Concentrated solution for rapid reduction type hydraulic support in low-temperature environment and preparation method thereof
1. A concentrated solution for a rapid reduction type hydraulic support in a low-temperature environment is prepared from the following components in parts by mass:
the total mass of all the components is 100 parts, wherein the polymeric amino acid accounts for 5-15 parts; 4-10 parts of a nonionic and anionic group composite coupling agent; 2-6 parts of an alcohol amine type buffering agent; 13-30 parts of organic and inorganic composite pour point depressant; 6.1-13.7 parts of a non-ferrous metal and ferrous metal composite corrosion inhibitor; 1-3 parts of a mould bacteria inhibitor; 1-3 parts of alcohol modified polyether; the balance being water.
2. The concentrate of claim 1, wherein: the nonionic and anionic group composite coupling agent is prepared from water, a nonionic coupling agent and an anionic coupling agent in a mass ratio of 5: 1.5-2.5: 2-4;
the nonionic and anionic group composite coupling agent is prepared by the following steps: mixing the water and the anionic coupling agent, and then adding the nonionic coupling agent for mixing.
3. The concentrate of claim 2, wherein: the non-ionic coupling agent comprises at least one of dipropylene glycol monomethyl ether, polycarbonate and triethylene glycol butyl ether;
the anionic coupling agent includes at least one of a sulfate salt, a carboxylate salt, and a sulfonate salt.
4. The concentrate of any of claims 1-3, wherein: the organic and inorganic composite pour point depressant is prepared from the following components in parts by mass: 15 parts of water; 5-10 parts of inorganic salt; 0-15 parts of a polyol;
the preparation method of the organic and inorganic composite pour point depressant comprises the following steps: adding the water, the inorganic salt and the polyol into a reaction kettle in sequence, mixing and stirring for reaction to obtain the organic and inorganic composite pour point depressant;
the reaction temperature is 60-80 ℃, the reaction time is 15-25 min, and the stirring rotation speed is 60-90 r/min;
the nonferrous metal and ferrous metal composite corrosion inhibitor comprises the following components in parts by mass: 0.7 part of triazole; 3-5 parts of aromatic acid salt, 3-9 parts of poly-tribasic carboxylic acid and 10-15 parts of ammonium salt solution.
5. The concentrate of claim 4, wherein: the inorganic salt comprises at least one of nitrate, molybdate and nitrite;
the polyol comprises at least one of ethylene glycol, polyethylene glycol and glycerol;
the triazole comprises at least one of triadimefon, triadimenol and benzotriazole; the aromatic acid salt comprises at least one of benzoate, phthalate and isophthalate; the poly-tricarboxylic acid comprises at least one of L190-B tricarboxylic acid, SYS50 tricarboxylic acid and triazine polycarboxylic acid rust inhibitor; the ammonium salt solution comprises at least one of alkylphenol polyoxyethylene ether ammonium sulfate salt, hydrolyzed polyacrylonitrile ammonium salt and ammonium dodecyl sulfate salt solution.
6. The concentrate of any of claims 1-5, wherein: the polymeric amino acid comprises at least one of polylysine, polyaspartic acid, and polyglutamic acid;
the alcohol amine type buffer includes at least one of triisopropanolamine, triethanolamine, and diethanolisopropanolamine;
the mold bacteria inhibitor comprises at least one of natamycin, octanoyl hydroxamic acid and isothiazolinone;
the alcohol-modified polyether comprises at least one of allyl alcohol polyoxyalkyl ether, fatty alcohol modified end-capped polyether and lauryl alcohol polyoxyethylene ether.
7. The method for preparing the concentrated solution for the rapid reduction type hydraulic support in the low-temperature environment of any one of claims 1 to 6, comprising the following steps: 1) sequentially adding the polymerized amino acid, the nonionic and anionic group composite coupling agent and the alcohol amine type buffering agent into water for mixing to obtain a mixed solution 1;
2) sequentially adding the organic and inorganic composite pour point depressant, the nonferrous metal and ferrous metal composite corrosion inhibitor into the mixed solution 1 for mixing to obtain a mixed solution 2;
3) and sequentially adding the mould bacteria inhibitor and the alcohol-modified polyether into the mixed solution 2 for mixing to obtain the concentrated solution for the rapid reduction type hydraulic support in the low-temperature environment.
8. The method of claim 7, wherein: the mixing conditions in step 1) were as follows: stirring and mixing; the temperature is 40-60 ℃, the stirring time is 20-40 min, and the stirring speed is 60-90 r/min.
9. The production method according to claim 7 or 8, characterized in that: the mixing conditions in step 2) were as follows: stirring and mixing; the temperature is 40-60 ℃, the stirring time is 30-50 min, and the stirring speed is 60-90 r/min.
10. The production method according to any one of claims 7 to 9, characterized in that: the mixing conditions in step 3) were as follows: stirring and mixing; the temperature is room temperature, the stirring time is 15-20 min, and the stirring speed is 60-90 r/min;
and step 3) also comprises the step of filling the concentrated solution for the rapid reduction type hydraulic support in the low-temperature environment into a storage tank, and filtering and filling to obtain a finished product.
Background
The transmission medium of the hydraulic support is known as the blood of the hydraulic support, and is of great importance to the stability and reliability of the operation of the hydraulic support in a coal mine. Generally, the high-water hydraulic fluid is classified into emulsified oil and concentrated liquid. The concentrated solution for the hydraulic bracket can be dissolved in water to form a liquid substance of solution type diluent. Generally comprises water, water-soluble antirust agent, anticorrosive agent, lubricant and other additives. The hydraulic support consists of high-water-content hydraulic liquid (oil-in-water emulsion prepared from emulsified oil and more than 95% of water or solution type diluent prepared from concentrated solution and more than 95% of water), an upright post, a jack, a control element, a top beam, a shield beam, a base and the like, and four basic actions of lifting, lowering, pushing and moving the support are realized mainly by means of the high-water-content hydraulic liquid, the upright post and the jack. The quality of emulsified oil or concentrated solution for the hydraulic support directly influences the action accuracy of the hydraulic support, and if abnormal phenomena (oil precipitation, soap precipitation, floccules, precipitates and jelly-like substances) which are difficult to recover after the high-water-content hydraulic fluid is condensed occur in winter, a pipeline system is blocked, the phenomenon of 'thrombus' occurs, and the safety, the efficiency and the high yield of a coal mine are influenced.
The hydraulic support concentrated solution is suitable for hydraulic equipment such as a hydraulic support, an externally-injected single hydraulic prop and the like, plays roles of lubrication, rust prevention and the like while transmitting power, and can provide effective protection for a hydraulic system. The hydraulic transmission medium is of great importance to the stability and reliability of the operation of the coal mine hydraulic support; in order to prevent the condensation phenomenon of a hydraulic support transmission medium in the process of transportation and storage (part of coal mines are stored in the open air or no heating facilities are arranged in a storehouse in winter), MT/T76-2011 'emulsified oil, concentrated solution and high-water-content hydraulic fluid for the hydraulic support' stipulates the freeze-thaw resistance of the hydraulic support transmission medium, a certain amount of samples are taken and put into a refrigerating device at the temperature of-21 ℃ to-16 ℃ for 8 hours, then taken out and put into the device at the temperature of 10 ℃ to 35 ℃ for 16 hours to serve as a freeze-thaw process, and after five cycles are repeated, the emulsified oil or the concentrated solution can be recovered to the original state. The emulsified oil or concentrated solution contains additives with different properties, such as lubricant, corrosion inhibitor, pour point depressant, buffering agent and the like, and the comprehensive action among the additives determines the recovery capability of the product after coagulation. Products with poor recovery capability seriously affect the pumping capacity of the products, and the phenomenon of pipeline blockage can be partially caused, so that the risk that concentrated solution or emulsified oil cannot be timely and automatically replenished is increased; aiming at the situation, a method of putting the product into the well in advance is usually adopted on the mine, and the product is quickly recovered by means of the temperature in the well; the invention adjusts the non-ionic and anionic composite coupling agent and uses with the composite pour point depressant, which makes the product system reduce quickly in low temperature environment after coagulating, and meets the requirement of using in winter of different mine products in different regions.
Disclosure of Invention
The invention aims to provide a concentrated solution for a rapid reduction type hydraulic support in a low-temperature environment and a preparation method thereof.
The invention provides a concentrated solution for a rapid reduction type hydraulic support in a low-temperature environment, which is prepared from the following components in parts by mass:
the total mass of all the components is 100 parts, wherein the polymeric amino acid accounts for 5-15 parts; 4-10 parts of a nonionic and anionic group composite coupling agent; 2-6 parts of an alcohol amine type buffering agent; 13-30 parts of organic and inorganic composite pour point depressant; 6.1-13.7 parts of a non-ferrous metal and ferrous metal composite corrosion inhibitor; 1-3 parts of a mould bacteria inhibitor; 1-3 parts of alcohol modified polyether; the balance being water.
In the invention, the concentrated solution for the rapid reduction type hydraulic support in the low-temperature environment is prepared from the following components in parts by mass in any one of A) to D):
A) the total mass part of all the components is 100 parts, wherein the total mass part is 15 parts of polymerized amino acid; 4 parts of nonionic and anionic group composite coupling agent; 2 parts of alcohol amine type buffering agent; 15 parts of organic and inorganic composite pour point depressant; 7.1 parts of a non-ferrous metal and ferrous metal composite corrosion inhibitor; 3 parts of a mould bacteria inhibitor; 1 part of alcohol modified polyether; the balance of water;
B) the total mass part of all the components is 100 parts, wherein the total mass part is 10 parts of polymerized amino acid; 7 parts of nonionic and anionic group composite coupling agent; 3 parts of an alcohol amine type buffering agent; 20 parts of organic and inorganic composite pour point depressant; 10.1 parts of a non-ferrous metal and ferrous metal composite corrosion inhibitor; 2 parts of a mould bacteria inhibitor; 2 parts of alcohol modified polyether; the balance of water;
C) the total mass parts of all the components are 100 parts, wherein 6 parts of polymeric amino acid, 10 parts of nonionic and anionic group composite coupling agent, 6 parts of alcohol amine type buffering agent, 30 parts of organic and inorganic composite pour point depressant, 13.7 parts of nonferrous metal and ferrous metal composite corrosion inhibitor, 1 part of mould bacteria inhibitor, 3 parts of alcohol modified polyether and the balance of water;
D) the total mass of all the components is 100 parts, wherein the total mass of all the components is 6-15 parts of polymerized amino acid; 4-10 parts of a nonionic and anionic group composite coupling agent; 2-6 parts of an alcohol amine type buffering agent; 15-30 parts of organic and inorganic composite pour point depressant; 7.1-13.7 parts of a non-ferrous metal and ferrous metal composite corrosion inhibitor; 1-3 parts of a mould bacteria inhibitor; 1-3 parts of alcohol modified polyether; the balance being water.
In the concentrated solution, the nonionic and anionic group composite coupling agent comprises water, a nonionic coupling agent and an anionic coupling agent in a mass ratio of 5: 1.5-2.5: 2-4, and specifically can be 5:2: 3;
the nonionic and anionic group composite coupling agent is prepared by the following steps: mixing the water and the anionic coupling agent, and then adding the nonionic coupling agent for mixing.
In the above concentrated solution, the non-ionic coupling agent comprises at least one of dipropylene glycol monomethyl ether, polycarbonate and triethylene glycol butyl ether;
the anion coupling agent comprises at least one of sulfate ester salt, carboxylate and sulfonate, and the cation of the anion coupling agent is common cation.
In the concentrated solution, the organic and inorganic composite pour point depressant is prepared from the following components in parts by mass: 15 parts of water; 5-10 parts of inorganic salt; 0-15 parts of a polyol; the paint can be prepared from 15 parts of water, 5 parts of inorganic salt and 10 parts of polyol;
the preparation method of the organic and inorganic composite pour point depressant comprises the following steps: adding the water, the inorganic salt and the polyol into a reaction kettle in sequence, mixing and stirring for reaction to obtain the organic and inorganic composite pour point depressant;
the reaction temperature is 60-80 ℃, the reaction time is 15-25 min, and the stirring rotation speed is 60-90 r/min;
the nonferrous metal and ferrous metal composite corrosion inhibitor comprises the following components in parts by mass: 0.7 part of triazole, 3-5 parts of aromatic acid salt, 3-9 parts of poly-tricarboxylic acid and 10-15 parts of ammonium salt solution; the aromatic water-based paint is specifically prepared from 0.7 part of triazole, 3 parts of aromatic acid salt, 9 parts of poly-tricarboxylic acid and 15 parts of ammonium salt solution.
In the concentrated solution, the inorganic salt comprises at least one of nitrate, molybdate and nitrite, and the cation of the inorganic salt is common ammonium, alkali metal, magnesium or thallium salt;
the polyol comprises at least one of ethylene glycol, polyethylene glycol and glycerol;
the triazole comprises at least one of triadimefon, triadimenol and benzotriazole; the aromatic acid salt comprises at least one of benzoate, phthalate and isophthalate, and the cation of the aromatic acid salt is common salt cation; the poly-tricarboxylic acid comprises at least one of L190-B tricarboxylic acid, SYS50 tricarboxylic acid and triazine polycarboxylic acid rust inhibitor; the ammonium salt solution comprises at least one of alkylphenol polyoxyethylene ether ammonium sulfate salt, hydrolyzed polyacrylonitrile ammonium salt and ammonium dodecyl sulfate salt solution.
In the above concentrated solution, the polymeric amino acid comprises at least one of polylysine, polyaspartic acid and polyglutamic acid;
the alcohol amine type buffer includes at least one of triisopropanolamine, triethanolamine, and diethanolisopropanolamine;
the mold bacteria inhibitor comprises at least one of natamycin, octanoyl hydroxamic acid and isothiazolinone;
the alcohol-modified polyether comprises at least one of allyl alcohol polyoxyalkyl ether, fatty alcohol modified end-capped polyether and lauryl alcohol polyoxyethylene ether.
The invention also provides a preparation method of the concentrated solution for the rapid reduction type hydraulic support in the low-temperature environment, which comprises the following steps: 1) sequentially adding the polymerized amino acid, the nonionic and anionic group composite coupling agent and the alcohol amine type buffering agent into water for mixing to obtain a mixed solution 1;
2) sequentially adding the organic and inorganic composite pour point depressant, the nonferrous metal and ferrous metal composite corrosion inhibitor into the mixed solution 1 for mixing to obtain a mixed solution 2;
3) and sequentially adding the mould bacteria inhibitor and the alcohol-modified polyether into the mixed solution 2 for mixing to obtain the concentrated solution for the rapid reduction type hydraulic support in the low-temperature environment.
In the above preparation method, the mixing conditions in step 1) are as follows: stirring and mixing; the temperature is 40-60 ℃, the stirring time is 20-40 min, and the stirring speed is 60-90 r/min.
In the above preparation method, the mixing conditions in step 2) are as follows: stirring and mixing; the temperature is 40-60 ℃, the stirring time is 30-50 min, and the stirring speed is 60-90 r/min.
In the above preparation method, the mixing conditions in step 3) are as follows: stirring and mixing; the temperature is room temperature, the stirring time is 15-20 min, and the stirring speed is 60-90 r/min;
and step 3) also comprises the step of filling the concentrated solution for the rapid reduction type hydraulic support in the low-temperature environment into a storage tank, and filtering and filling to obtain a finished product.
In the invention, the concentrated solution for the rapid reduction type hydraulic support in the low-temperature environment is condensed at low temperature (-45 ℃) and then is placed for 2 to 5 hours at the temperature of-15 to 0 ℃, and the concentrated solution for the rapid reduction type hydraulic support in the low-temperature environment can be recovered.
The invention has the following advantages:
the raw materials are added with the nonionic and anionic group composite coupling agent and are matched with the composite pour point depressant for use, so that a product system can be quickly reduced in a low-temperature environment after being condensed, the addition amount of the raw materials has a certain elastic range, and on the basis of meeting the requirements of lubrication, rust prevention and corrosion prevention, the product can be quickly reduced in the environment of-15-0 ℃ after being condensed at a low temperature by adjusting the proportion of the nonionic and anionic group composite coupling agent to the pour point depressant; the pumping capacity of the product is improved, the product is guaranteed to be automatically supplemented with the concentrated solution, and the advantages are more prominent in the use in the northwest and northeast coal mines in winter. The customized product according to the invention can ensure that the liquid supply of the hydraulic support is more reliable, and is beneficial to intelligent mine construction.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The first embodiment,
The concentrated solution for the rapid reduction type hydraulic support in the low-temperature environment comprises 100 parts of preparation components in parts by mass, wherein the preparation components comprise the following raw materials in parts by mass: 15 parts of polymeric amino acid (polylysine and polyaspartic acid are mixed according to the mass ratio of 1: 1), 4 parts of nonionic and anionic group composite coupling agent, 2 parts of alcohol amine type buffer (triisopropanolamine and triethanolamine are mixed according to the mass ratio of 1: 1), 15 parts of organic and inorganic composite pour point depressant, 7.1 parts of nonferrous metal and ferrous metal composite corrosion inhibitor, 3 parts of mould bacteria inhibitor (natamycin and isothiazolinone are mixed according to the mass ratio of 1: 1), 1 part of alcohol modified polyether (allyl alcohol polyoxyalkyl ether), and the balance of water.
In this example, the nonionic and anionic group composite coupling agent: the mass ratio of water to the non-ionic coupling agent (dipropylene glycol monomethyl ether) to the anionic coupling agent (sodium carboxylate) is 5:2:3, and the components are stirred and mixed at normal temperature until the components are uniform and bright.
In the embodiment, for the preparation of the organic and inorganic composite pour point depressant, 15 parts of water, 5 parts of inorganic salt (sodium nitrate and sodium molybdate are mixed according to the mass ratio of 1: 1) and 10 parts of polyol (ethylene glycol and polyethylene glycol are mixed according to the mass ratio of 1: 1) are sequentially added into a reaction kettle, the reaction temperature is controlled at 60 ℃, the stirring is carried out for 15min, and the rotating speed is 60r/min, so that the uniform and transparent organic and inorganic composite pour point depressant is obtained.
In this embodiment, the nonferrous metal and ferrous metal composite corrosion inhibitor includes 0.7 parts of triazole (triazolone and benzotriazole are mixed according to a mass ratio of 1: 1), 3 parts of aromatic acid salt (sodium benzoate), 9 parts of poly-tribasic carboxylic acid (L190-B tribasic polycarboxylic acid), and 15 parts of ammonium salt solution (alkylphenol polyoxyethylene ether ammonium sulfate).
In this example, the specific preparation method of the concentrated solution comprises the following steps:
1) preparing a nonionic and anionic group composite coupling agent; sequentially adding water, an anionic coupling agent and a nonionic coupling agent, stirring for 10min at normal temperature (25 ℃) to obtain a composite coupling agent, and sampling and observing to obtain a uniform and transparent liquid.
2) Adding a proper amount of water into a reaction kettle, sequentially adding 15 parts of polymerized amino acid, 4 parts of nonionic and anionic group composite coupling agent and 2 parts of alcohol amine type buffering agent into the water, stirring for 20min at 40 ℃, rotating at 60r/min to obtain a mixed solution 1, and sampling and observing to obtain a uniform and transparent liquid.
3) Adding an organic and inorganic composite pour point depressant; and (2) sequentially adding 15 parts of organic and inorganic composite pour point depressant, 7.1 parts of nonferrous metal and ferrous metal composite corrosion inhibitor into the mixed solution 1, stirring for 30min at 40 ℃ and at the rotating speed of 60r/min to obtain a mixed solution 2, and sampling and observing to ensure that the liquid is uniform and transparent.
4) Sequentially adding 3 parts of a mould bacteria inhibitor and 1 part of alcohol-modified polyether into the mixed solution 2, stirring for 15min under natural conditions (25 ℃, without temperature rise and drop operation), rotating at the speed of 60r/min to obtain a concentrated solution for the rapid reduction type hydraulic support in a low-temperature environment, and sampling and observing to ensure that the liquid is uniform and transparent;
5) and (3) pumping the concentrated solution obtained in the step 4) into a storage tank, filtering and filling, and marking as a No. I product.
In this example, after the concentrated solution i for a low-temperature rapid reduction type hydraulic stent and the similar products (control group) on the market are respectively coagulated at a low temperature (-45 ℃), the products are uniformly placed under an environment condition of 0 ℃, and observed once per hour, the time required for product recovery (no delamination, no oil precipitation, no soap precipitation, no floc, no sediment, no jelly-like substance) is observed and recorded, when the recovery time is more than 8 hours, the recovery time is uniformly recorded as 9 hours, after five cycles are repeated, the average value of the recovery time is taken and recorded as the recovery time, and the recovery time is shown in table 1, and the lubricity, the rust resistance and the corrosion resistance of the products are measured at the same time.
In Table 1, control group I, control group II and control group III are commercially available products and used as control groups.
As can be seen from Table 1, the lubricating property, the rust resistance and the corrosion resistance of the product I of the invention and the products (a control group I, a control group II and a control group III) sold in the market at present meet the technical requirements, and the lubricating property is relatively excellent; under the low-temperature environment of-15-0 ℃, the recovery time of the product I is obviously shorter than that of the current commercial product, mainly because the formula of the product adopts a compounding and synergistic technology of 'polymerized amino acid + nonionic and anionic compound coupling + organic and inorganic compound pour point depressing'.
TABLE 1 comparison of the coagulation reduction times of product No. I, a low-temperature rapid-reduction concentrate, and commercial products
Example II,
The concentrated solution for the rapid reduction type hydraulic support in the low-temperature environment comprises 100 parts of preparation components in parts by mass, wherein the preparation components comprise the following raw materials in parts by mass: 10 parts of polymeric amino acid (polyaspartic acid and polyglutamic acid are mixed according to the mass ratio of 1: 1), 7 parts of nonionic and anionic group composite coupling agent, 3 parts of alcohol amine type buffer (triethanolamine and diethanol monoisopropanolamine are mixed according to the mass ratio of 1: 1), 20 parts of organic and inorganic composite pour point depressant, 10.1 parts of nonferrous metal and ferrous metal composite corrosion inhibitor, 2 parts of mould bacteria inhibitor (caprylyl hydroxamic acid and isothiazolinone are mixed according to the mass ratio of 1: 1), 2 parts of alcohol modified polyether (specifically fatty alcohol modified capped polyether which is commercially available from Shanghai Jiang Yong Engyi Limited company, the product number is CF-18), and the balance of water.
In this example, the mass ratio of the nonionic and anionic group composite coupling agent, water, the nonionic coupling agent (polycarbonate and triethylene glycol butyl ether mixed in a mass ratio of 1: 1) and the anionic coupling agent (sodium carboxylate and sodium sulfonate mixed in a mass ratio of 1: 1) was 5:2:3, and the mixture was stirred and mixed at room temperature until it was uniformly clear.
In this example, for the preparation of the organic and inorganic composite pour point depressant, 15 parts of water, 8 parts of inorganic salt (sodium molybdate and sodium nitrite are mixed according to a mass ratio of 1: 1), and 12 parts of polyol (ethylene glycol and glycerol are mixed according to a mass ratio of 1: 1) are sequentially added into a reaction kettle, the reaction temperature is controlled at 70 ℃, the stirring is carried out for 20min, and the rotating speed is 70r/min, so as to obtain the uniform and transparent organic and inorganic composite pour point depressant.
In the embodiment, the non-ferrous metal and ferrous metal composite corrosion inhibitor comprises 0.7 part of triazole (triazole and benzotriazole are mixed according to a mass ratio of 1: 1), 4 parts of aromatic acid salt (sodium phthalate), 6 parts of poly (tricarboxylic acid) (SYS 50) and 12 parts of ammonium salt solution (hydrolyzed polyacrylonitrile ammonium).
In this example, the specific preparation method of the concentrated solution comprises the following steps:
1) preparing a nonionic and anionic group composite coupling agent; and sequentially adding water, an anionic coupling agent and a nonionic coupling agent, stirring for 15min at normal temperature respectively to obtain a composite coupling agent, and sampling and observing to obtain a uniform and transparent liquid.
2) Adding a proper amount of water into a reaction kettle, sequentially adding 10 parts of polymerized amino acid, 7 parts of nonionic and anionic group composite coupling agent and 3 parts of alcohol amine type buffering agent into the water, stirring for 30min at 50 ℃, rotating at 70r/min to obtain a mixed solution 1, and sampling and observing to obtain a uniform and transparent liquid.
3) Adding an organic and inorganic composite pour point depressant; sequentially adding 20 parts of organic and inorganic composite pour point depressant, 10.1 parts of nonferrous metal and ferrous metal composite corrosion inhibitor into the mixed solution 1, stirring at 50 ℃ for 40min at a rotating speed of 70r/min to obtain a mixed solution 2, and sampling and observing to obtain a uniform and transparent liquid.
4) Sequentially adding 2 parts of mould bacteria inhibitor and 2 parts of alcohol modified polyether into the mixed solution 2, stirring for 15min under natural conditions (25 ℃) (without temperature rise and drop operation), rotating at 70r/min to obtain concentrated solution, and sampling and observing to obtain uniform and transparent liquid;
5) and (3) pumping the concentrated solution obtained in the step (4) into a storage tank, filtering and filling, and marking as a No. II product.
In this example, after the concentrated solution ii for the low-temperature rapid reduction type hydraulic stent and the similar products (control group) on the market are respectively coagulated at a low temperature (-45 ℃), the products are uniformly placed at-5 ℃ and observed once per hour, the time required for recovering the products (no delamination, no oil separation, no soap separation, no floc, no precipitate, no jelly-like substance) is observed and recorded, when the recovery time is more than 8 hours, the recovery time is uniformly recorded as 9 hours, after five cycles are repeated, the average value of the recovery time is taken and recorded as the recovery time, and the lubricity, the rust resistance and the corrosion resistance of the products are measured at the same time as shown in table 2.
As can be seen from Table 2, the lubricating property, the rust resistance and the corrosion resistance of the product II of the invention and the products (a comparison group I, a comparison group II and a comparison group III) sold in the market at present meet the technical requirements, and the lubricating property is the same as that of the comparison group III and is relatively better; under the low-temperature environment of-15 ℃ to 0 ℃, the recovery time of the product II is obviously shorter than that of the current commercial product, mainly because the product formula adopts a compound synergistic technology of 'polymerized amino acid + nonionic and anionic compound coupling + organic and inorganic compound pour point depressing', and the product II contains relatively more nonionic and anionic compound coupling agents, thereby further promoting the rapid recovery at low temperature.
TABLE 2 comparison of the coagulation reduction times of product II, a low-temperature rapid-reduction concentrate, and commercially available products
Example III,
The concentrated solution for the rapid reduction type hydraulic support in the low-temperature environment comprises 100 parts of total mass, wherein the raw materials comprise: 6 parts of polymeric amino acid (polylysine and polyglutamic acid are mixed according to the mass ratio of 1: 1), 10 parts of nonionic and anionic group composite coupling agent, 6 parts of alcohol amine type buffering agent (triethanolamine and diethanol monoisopropanolamine are mixed according to the mass ratio of 1: 1), 30 parts of organic and inorganic composite pour point depressant, 13.7 parts of nonferrous metal and ferrous metal composite corrosion inhibitor, 1 part of mould bacteria inhibitor (natamycin and caprylyl hydroxamic acid are mixed according to the mass ratio of 1: 1), 3 parts of alcohol modified polyether (dodecyl alcohol polyoxyethylene ether), and the balance of water.
In this example, the mass ratio of the nonionic coupling agent to the anionic coupling agent (dipropylene glycol monomethyl ether and triethylene glycol butyl ether mixed at a mass ratio of 1: 1) to the anionic coupling agent (sodium carboxylate and sodium sulfonate mixed at a mass ratio of 1: 1) was 5:2:3, and the mixture was stirred and mixed at room temperature (25 ℃) until the mixture was uniform and clear.
In the embodiment, the preparation of the organic and inorganic composite pour point depressant is carried out by sequentially adding 15 parts of water, 10 parts of inorganic salt (sodium nitrate, sodium molybdate and sodium nitrite are mixed according to the mass ratio of 1:1: 1) and 15 parts of polyol (ethylene glycol, polyethylene glycol and glycerol are mixed according to the mass ratio of 1:1: 1) into a reaction kettle, controlling the reaction temperature at 80 ℃, stirring for 25min and rotating at 90r/min to obtain the uniform and transparent organic and inorganic composite pour point depressant.
In this embodiment, the nonferrous metal and ferrous metal composite corrosion inhibitor includes 0.7 part of triazole (triazolone, triadimenol and benzotriazole are mixed according to a mass ratio of 1:1: 1), 5 parts of aromatic acid salt (sodium isophthalate), 3 parts of poly-tricarboxylic acid (triazine polycarboxylic acid antirust agent) and 10 parts of ammonium salt solution (ammonium dodecyl sulfate).
In this example, the specific preparation method of the concentrated solution comprises the following steps:
1) preparing a nonionic and anionic group composite coupling agent; and sequentially adding water, an anionic coupling agent and a nonionic coupling agent, stirring for 15min at normal temperature respectively to obtain a composite coupling agent, and sampling and observing to obtain a uniform and transparent liquid.
2) Adding a proper amount of water into a reaction kettle, sequentially adding 6 parts of polymerized amino acid, 10 parts of nonionic and anionic group composite coupling agent and 6 parts of alcohol amine type buffering agent into the water, stirring for 40min at the temperature of 60 ℃, rotating at the speed of 90r/min to obtain a mixed solution 1, and sampling and observing to obtain a uniform and transparent liquid.
3) Adding an organic and inorganic composite pour point depressant; and sequentially adding 30 parts of organic and inorganic composite pour point depressant, 13.7 parts of nonferrous metal and ferrous metal composite corrosion inhibitor into the mixed solution 1, stirring for 50min at the temperature of 60 ℃, rotating at the speed of 90r/min to obtain a mixed solution 2, and sampling and observing to obtain a uniform and transparent liquid.
4) Sequentially adding 1 part of mould bacteria inhibitor and 3 parts of alcohol-modified polyether into the mixed solution 2, stirring for 20min under natural conditions (without temperature rise and drop operation), rotating at the speed of 90r/min to obtain a concentrated solution, and sampling and observing to obtain a uniform and transparent liquid;
5) and (3) pumping the concentrated solution obtained in the step (4) into a storage tank, filtering and filling, and marking as a No. III product.
In this example, after the concentrated solution iii for the low-temperature rapid reduction type hydraulic stent and the similar products (control group) on the market were respectively coagulated at a low temperature (-45 ℃), the products were uniformly placed at-15 ℃ and observed once per hour, the time required for the recovery of the products (no delamination, no oil separation, no soap separation, no floc, no precipitate, no jelly-like substance) was observed and recorded, when the recovery time was > 8 hours, the time was uniformly recorded as 9 hours, after repeating five cycles, the average value of the recovery times was taken and recorded as the recovery time, and the lubricity, rust resistance and corrosion resistance of the products were measured at the same time as shown in table 3.
As can be seen from Table 3, the lubricating property, rust resistance and corrosion resistance of the product III of the invention and the currently marketed products (the control group I, the control group II and the control group III) all meet the technical requirements, and the lubricating property is at a medium level; under the low-temperature environment of-15 ℃ to 0 ℃, the recovery time of the product III is obviously shorter than that of the current commercial product, mainly because the product formula adopts a compound synergistic technology of 'polymerized amino acid + nonionic and anionic composite coupling + organic and inorganic composite pour point depressant', and the nonionic and anionic composite coupling agent + organic and inorganic composite pour point depressant in the product III are relatively more, so that the quick recovery at low temperature is kept.
TABLE 3 comparison of the coagulation reduction times of product No. III, a low-temperature rapid-reduction concentrate, with those of a commercial product
According to the first, second and third embodiments, the low-temperature rapid reduction type concentrated solution is obtained respectively, and the similar products on the market are taken as a control group. As can be seen from tables 1, 2 and 3, the concentrated solution for the low-temperature rapid reduction type hydraulic product I, product II and product III brackets can be restored after being condensed at low temperature (-45 ℃) and placed for 2 to 5 hours under the environment condition of-15 ℃ to 0 ℃ on the basis of meeting the requirements of lubrication, rust prevention and corrosion prevention, and the restoration time is obviously shorter than that of the current commercial products (a control group I, a control group II and a control group III).
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
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