1. A production method of an auxiliary agent potassium phosphate for short fiber production is characterized in that: the preparation method comprises the following steps:

(1) preparation of alkaline water: adding soft water into an alkali kettle reaction tank, adding potassium hydroxide, starting a stirrer in the alkali kettle tank, stirring for 40-50 min, starting an alkali water pump for circulation treatment for 20-25 min, and sampling to adjust the pH value of alkali water to 6.25-6.30;

(2) preparation of phosphate ester: adding fatty alcohol into a phosphorus kettle, heating to 42-45 ℃ in a steam heating mode, starting a stirrer in the phosphorus kettle, stirring for 30-40 min, heating to 60-65 ℃, adding distilled water with the same temperature, slowly adding phosphorus pentoxide powder in a continuously stirring state, heating to 88-89 ℃, keeping the temperature for 3-4 h, cooling to 74-85 ℃, adding hydrogen peroxide, continuously stirring, cooling to 68-70 ℃, and stopping stirring; the amount of the distilled water is 3-5% of the weight of the phosphorus pentoxide powder;

(3) respectively filtering the materials prepared in the step (1) h and the step (2), then sending the filtered materials into a comprehensive kettle, starting a stirrer in the comprehensive kettle, uniformly stirring, reacting at a constant temperature of 53-55 ℃ for 5-5.5 h, then adjusting the pH value, finally cooling to 33-35 ℃, and then filling.

2. The method for producing the potassium phosphate salt used as the auxiliary agent for producing the short fibers according to claim 1, is characterized in that: the dosage ratio of the soft water to the potassium hydroxide is 2300 multiplied by 10 by weight³－2350×10³：320－330。

3. The method for producing the potassium phosphate salt used as the auxiliary agent for producing the short fibers according to claim 1, is characterized in that: the frequency of the stirrer in the phosphorus kettle is 59HZ, and the frequency of the stirrer in the comprehensive kettle is 44 HZ.

4. The method for producing the potassium phosphate salt used as the auxiliary agent for producing the short fibers according to claim 1, is characterized in that: the dosage ratio of the fatty alcohol to the phosphorus pentoxide powder and the hydrogen peroxide is 1000-: 500-600: 2.5-5.

5. the method for producing the potassium phosphate salt used as the auxiliary agent for producing the short fibers according to claim 1, is characterized in that: the materials prepared in the step (1) and the step (2) are prepared according to the formula of 2200-: 1300 plus 1350 weight ratio into the comprehensive kettle.

6. The method for producing the potassium phosphate salt used as the auxiliary agent for producing the short fibers according to claim 1, is characterized in that: the pH value is adjusted by alkaline water.

7. The method for producing the potassium phosphate salt used as the auxiliary agent for producing the short fibers according to claim 1, is characterized in that: the cooling adopts a mode of introducing cooling water.

8. The method for producing the potassium phosphate salt used as the auxiliary agent for producing the short fibers according to claim 1, is characterized in that: the fatty alcohol is dodecanol.

9. The method for producing the potassium phosphate salt used as the auxiliary agent for producing the short fibers according to claim 1, is characterized in that: the fatty alcohol is stearyl alcohol.

10. The method for producing the potassium phosphate salt used as the auxiliary agent for producing the short fibers according to claim 1, is characterized in that: the fatty alcohol is composed of dodecanol and octadecanol according to a weight ratio of 2: 1, mixing the mixture.

Background

The potassium phosphate is the main component of short fiber oil, the oil prepared by the potassium phosphate can make short fiber have good antistatic property, smoothness and proper cohesive property (i.e. bundling property), phosphorus pentoxide commonly used in industry reacts with higher fatty alcohol to obtain phosphate, then the phosphate is neutralized with KOH aqueous solution to form salt, unreacted raw material alcohol and a small amount of polyester and other impurities are also contained in reaction products besides the potassium phosphate, because the reaction of fatty alcohol and phosphorus pentoxide belongs to exothermic reaction, if the reaction temperature is not well controlled, the fatty alcohol is easily carbonized, the finally obtained phosphate has low purity and poor color, and the performance of the phosphate has direct influence on the performance of the final product potassium phosphate.

Due to different preparation raw materials, preparation process parameters and the like, the potassium monoester-diester phosphate with different proportions can be obtained, the potassium diester phosphate has better smoothness and oleophylic property, but the antistatic property is poorer, and the monoester has better hydrophilicity, antistatic property and foaming property, so that the higher the monoester content is, the better the antistatic property is.

Chinese patent application No. 200910307707.6 discloses a method for preparing high-stability potassium alkyl phosphate emulsion, which comprises the following steps: (1) stirring the potassium hydroxide solution at the speed of 250-300 rpm for 30-60 min, and ultrasonically oscillating the alkyl phosphate for 3-10 min; (2) dropping appropriate amount of alkyl phosphate into the potassium hydroxide solution under stirring, and reacting at 65-70 deg.C for 30 min; (3) the invention claims that the prepared potassium alkyl phosphate salt has high stability when the pH is adjusted to 10 ± 1 with potassium hydroxide solution and cooled to room temperature, but the disclosed method is too simple to actually achieve the technical effects described.

Disclosure of Invention

Therefore, aiming at the problems, the invention provides a production method of an auxiliary agent potassium phosphate for short fiber production, which solves the defects of low purity, poor antistatic property and unsuitable cohesive property of the potassium phosphate prepared by the preparation method in the prior art.

In order to achieve the purpose, the invention adopts the following technical scheme: a production method of an auxiliary agent potassium phosphate for short fiber production comprises the following preparation methods:

(1) preparation of alkaline water: adding soft water into an alkali kettle reaction tank, adding potassium hydroxide, starting a stirrer in the alkali kettle tank, stirring for 40-50 min, starting an alkali water pump for circulation treatment for 20-25 min, and sampling to adjust the pH value of alkali water to 6.25-6.30;

(2) preparation of phosphate ester: adding fatty alcohol into a phosphorus kettle, heating to 42-45 ℃ in a steam heating mode, starting a stirrer in the phosphorus kettle, stirring for 30-40 min, heating to 60-65 ℃, adding distilled water with the same temperature, slowly adding phosphorus pentoxide powder in a continuously stirring state, heating to 88-89 ℃, keeping the temperature for 3-4 h, cooling to 74-85 ℃, adding hydrogen peroxide, continuously stirring, cooling to 68-70 ℃, and stopping stirring; the amount of the distilled water is 3-5% of the weight of the phosphorus pentoxide powder;

(3) respectively filtering the materials prepared in the step (1) h and the step (2), then sending the filtered materials into a comprehensive kettle, starting a stirrer in the comprehensive kettle, uniformly stirring, reacting at a constant temperature of 53-55 ℃ for 5-5.5 h, then adjusting the pH value, finally cooling to 33-35 ℃, and then filling.

The further improvement is that: the dosage ratio of the soft water to the potassium hydroxide is 2300 multiplied by 10 by weight³－2350×10³：320－330。

The further improvement is that: the frequency of the stirrer in the phosphorus kettle is 59HZ, and the frequency of the stirrer in the comprehensive kettle is 44 HZ.

The further improvement is that: the dosage ratio of the fatty alcohol to the phosphorus pentoxide powder and the hydrogen peroxide is 1000-: 500-600: 2.5-5.

the further improvement is that: the materials prepared in the step (1) and the step (2) are prepared according to the formula of 2200-: 1300 plus 1350 weight ratio into the comprehensive kettle.

The further improvement is that: the pH value is adjusted by alkaline water.

The further improvement is that: the cooling adopts a mode of introducing cooling water.

The further improvement is that: the fatty alcohol is dodecanol.

The further improvement is that: the fatty alcohol is composed of dodecanol and octadecanol according to a weight ratio of 2: 1, mixing the mixture.

By adopting the technical scheme, the invention has the beneficial effects that:

1. in the preparation process of the phosphate, a small amount of distilled water is added into the phosphorus kettle, and the small amount of water reacts with the phosphorus pentoxide to generate the phosphoric acid, so that the caking phenomenon of the phosphorus pentoxide is weakened, the uniform dispersion of the phosphorus pentoxide is facilitated, and the esterification reaction is promoted.

2. The adding amount of distilled water in the phosphorus kettle is controlled to be 3-5% of the weight of phosphorus pentoxide powder, which is beneficial to the generation of monoester, and if the adding amount is higher than 5%, the adding amount of phosphoric acid is too high, which hinders the generation of monoester.

3. In the preparation process of the phosphate, the phosphorus pentoxide powder is slowly added, the reaction temperature is controlled to 88-89 ℃, the temperature is kept constant for 3-4 h, the amount of the monoester obtained under the condition reaches 90%, the reaction speed is high due to the fact that the concentrations of phosphorus pentoxide and fatty alcohol in a reaction kettle are high at the beginning, but the concentrations of the fatty alcohol and the phosphorus pentoxide are weakened along with the reaction, and the reaction reaches the balance in about 4h through tests under the condition that the raw material amount is not increased.

4. In the preparation process of the phosphate, the reaction temperature is controlled to be 88-89 ℃, the reaction speed is high in the temperature range, the monoester is not easy to carbonize, the color of the product is light, the monoester is not subjected to hydrolysis reaction, and the monoester with high content can be obtained.

5. The monoester obtained by the preparation method has high content, and because the monoester contains two hydrophilic groups, the monoester is easy to dissolve in water and has good hygroscopicity, the monoester can be used on short fibers to ensure that the short fibers have better antistatic property and better bundling property.

6. The fatty alcohol is octadecanol or the fatty alcohol is dodecanol or the fatty alcohol and the octadecanol are mixed according to the proportion of 2: the mixture mixed by the weight ratio of 1 has better hygroscopicity due to the fact that dodecanol or octadecanol has a proper hydrophobic group chain, and therefore the prepared final product has better antistatic property.

Drawings

FIG. 1 is a schematic view of a stirrer inside a phosphorus kettle according to an embodiment of the present invention;

FIG. 2 is a schematic structural diagram of a stirring spindle according to a first embodiment of the present invention;

fig. 3 is a schematic structural diagram of a mixing spindle and a main mixing blade according to a first embodiment of the present invention.

Detailed Description

The invention will now be further described with reference to specific embodiments.

Example one

A production method of an auxiliary agent potassium phosphate for short fiber production comprises the following preparation methods:

(1) preparation of alkaline water: adding soft water 2320m3 into an alkali kettle reaction tank, adding 325kg of potassium hydroxide, opening a stirrer in the alkali kettle reaction tank, stirring for 40min, starting an alkali water pump for circulation treatment for 20min, and sampling to adjust the pH value of alkali water to 6.25;

(2) preparation of phosphate ester: adding 1100kg of dodecanol into a phosphorus kettle, starting steam to heat to 43 ℃, starting a stirrer in the phosphorus kettle, controlling the frequency of the stirrer to be 59HZ, then heating to 60 ℃ (controlling the temperature by closing the steam and starting cooling water after heating to 57 ℃), adding 25kg of distilled water with the same temperature, slowly adding 500kg of phosphorus pentoxide powder, closing the cooling water after the temperature rises to 74 ℃, starting the steam to heat when the temperature reaches 81 ℃, closing the steam when the temperature reaches 88 ℃, keeping the temperature for 3.5h, starting the cooling water to cool after 3.5h, cooling the temperature to about 103 ℃, adding 5kg of hydrogen peroxide after cooling to 85 ℃, closing the cooling water after cooling to 74 ℃, and stopping stirring after the temperature falls to 68 ℃;

(3) respectively filtering the materials prepared in the step (1) h and the step (2), then sending the filtered materials into a comprehensive kettle, starting a stirrer in the comprehensive kettle, uniformly stirring the materials at the stirrer frequency of 44HZ at a constant temperature of 53 ℃ for 5h, then adjusting the pH value, adjusting the pH value by adopting a potassium hydroxide aqueous solution, finally cooling to 33 ℃, and then filling.

Referring to fig. 1 to 3, a cover body 2 is arranged on the phosphorus kettle tank 1, a stirrer in the phosphorus kettle tank 1 comprises a stirring main shaft 4 and a stirring auxiliary shaft 5, one end of the stirring main shaft 4 penetrates out of the cover body 2 to be connected with a driving motor 3, the other end of the stirring main shaft extends into the phosphorus kettle tank 1 and is provided with a main stirring blade, the main stirring blade is formed by a first arc-shaped blade 61 and a second arc-shaped blade 62 which are distributed at intervals along the longitudinal direction, the first arc-shaped blade 61 is formed by two concentric arc-shaped blades 61a and 61b with different orientation radiuses, the second arc-shaped blade 62 and the first arc-shaped blade 61 are arranged in axial symmetry by taking the stirring main shaft 4 as a symmetry axis, namely, the second arc-shaped blade 62 is formed by two concentric arc-shaped blades 62a and 62b with different orientation radiuses, through holes 63 are uniformly distributed on the first arc-shaped blade 61, the radius of the through holes 63 is 2cm, the through holes have small radius and can allow liquid to pass through, the arrangement of the through hole can reduce the resistance during stirring, so that the stirring efficiency is higher, one end of the auxiliary stirring shaft 5 penetrates out of the cover body 2 and is connected with the driving motor 3 through the connecting rod 7, the other end extends into the stirring tank body 1 and is provided with an auxiliary stirring blade 8, the auxiliary stirring blade 8 consists of a first stirring sheet 81 and a second stirring sheet 82 which are connected in sequence, the included angle between the first stirring sheet 81 and the second stirring sheet 82 is 90 degrees, the stirring main shaft 4 is formed by detachably connecting a first stirring main shaft 41 and a second stirring main shaft 42, specifically, by arranging a reset hole on the first stirring main shaft, a return spring 44 and a return ball 43 are arranged in the second stirring main shaft 42, the return ball 43 is arranged on the return spring 44, and when the second stirring main shaft is connected, the return ball 43 is arranged in a return hole, by pressing the reset bead 43, the first stirring main shaft 41 and the second stirring main shaft 42 can be detachably connected.

The stirring main shaft of the stirrer in the phosphorus kettle tank is of a detachable structure, so that the stirrer is convenient to maintain and clean; the stirring tank is internally provided with a stirring main shaft and a stirring auxiliary shaft, the main shaft and the auxiliary shaft are both provided with stirring blades, the main shaft and the auxiliary shaft are combined for stirring, the stirring uniformity and efficiency are improved, moreover, the main stirring blades on the stirring main shaft are blades with arc structures, the blades are provided with through holes, the radius of the through holes is small but liquid can pass through, and the through holes can reduce the resistance during stirring, so that the stirring efficiency is higher; vice stirring vane comprises first stirring piece and second stirring piece and the contained angle between them is 30-90, makes the thick liquids stir by vice stirring vane once more after main stirring vane stirs, increases the homogeneity of stirring, and first stirring vane and second stirring vane's contained angle makes two blades enclose into a right angle or acute angle in specific range, can be to the great shearing force of thick liquids glueing, makes the material dispersed more evenly.

Example two

(1) Preparation of alkaline water: adding soft water 2300m3 into an alkali kettle reaction tank, adding potassium hydroxide 320kg, opening a stirrer in the alkali kettle tank, stirring for 40min, starting an alkali water pump for circulation treatment for 20min, and sampling to adjust the pH value of the alkali water to 6.25;

(2) preparation of phosphate ester: adding 1100kg of dodecanol into a phosphorus kettle, starting steam to heat to 43 ℃, starting a stirrer in the phosphorus kettle, controlling the frequency of the stirrer to be 59HZ, then heating to 62 ℃ (controlling the temperature by closing the steam and starting cooling water after heating to 57 ℃), adding 25kg of distilled water with the same temperature, slowly adding 520kg of phosphorus pentoxide powder, closing the cooling water after the temperature is increased to 75 ℃, starting the steam to heat when the temperature reaches 80 ℃, closing the steam when the temperature reaches 88 ℃, keeping the temperature for 4h, starting the cooling water to cool after 3.5h, cooling to 80 ℃ at 105 ℃, adding 5kg of hydrogen peroxide after cooling to 80 ℃, closing the cooling water after the temperature is reduced to 74 ℃, and stopping stirring after the temperature is reduced to 68 ℃;

(3) mixing the materials prepared in the step (1) h and the step (2) according to the proportion of 2200: respectively filtering the materials according to the weight ratio of 1300, sending the materials into a comprehensive kettle, starting a stirrer in the comprehensive kettle, uniformly stirring the materials at the frequency of 44HZ, carrying out constant-temperature reaction for 5 hours at the temperature of 53 ℃, then adjusting the pH value, adopting a potassium hydroxide aqueous solution for adjustment, finally cooling to 33 ℃, and then filling.

EXAMPLE III

(1) Preparation of alkaline water: adding soft water 2350m3 into an alkali kettle reaction tank, adding potassium hydroxide 330kg, opening a stirrer in the alkali kettle tank, stirring for 40min, starting an alkali water pump for circulation treatment for 20min, and sampling to adjust the pH value of alkali water to 6.3;

(2) preparation of phosphate ester: adding 1100kg of dodecanol into a phosphorus kettle, starting steam to heat to 43 ℃, starting a stirrer in the phosphorus kettle, controlling the frequency of the stirrer to be 59HZ, then heating to 60 ℃ (controlling the temperature by closing the steam and starting cooling water after heating to 57 ℃), adding 25kg of distilled water with the same temperature, slowly adding 500kg of phosphorus pentoxide powder, closing the cooling water after the temperature rises to 74 ℃, starting the steam to heat when the temperature reaches 81 ℃, closing the steam when the temperature reaches 88 ℃, keeping the temperature for 3.5h, starting the cooling water to cool after 3.5h, cooling the temperature to about 103 ℃, adding 2.5kg of hydrogen peroxide after cooling to 74 ℃, closing the cooling water after cooling to 71 ℃, and stopping stirring after the temperature is reduced to 68 ℃;

(3) filtering the materials prepared in the step (1) h and the step (2) respectively, and then performing mixing according to a ratio of 2300: 1350 weight percentages are sent into the comprehensive kettle and sent into the comprehensive kettle, a stirrer in the comprehensive kettle is started, the frequency of the stirrer is 44HZ, the stirring is uniform, the reaction is carried out for 5 hours at a constant temperature of 53 ℃, then the pH value is adjusted, the adjustment is carried out by adopting a potassium hydroxide aqueous solution, and finally the filling is carried out after the temperature is reduced to 33 ℃.

The products prepared in the first and second embodiments of the present invention were tested, and the results were as follows:

description of the test samples:

sample number SGS sample ID description

SN1 (example one) SHA-18-260618.001 white liquid

SN2 (example two) SHA-18-260618.002 yellow liquid

Remarking:

(1)1mg/kg＝0.0001％

(2) MDL (medium density language) method detection limit

(3) ND is not detected (< MDL)

(4) "-" is not specified

Octyl phenol polyoxyethylene ether (OPEOS), nonyl phenol polyoxyethylene ether (NPEOs)

The test method comprises the following steps: solvent extraction and analysis by HPLC-MS.

Remarking: (1) NPEOs reference information: 1907/2006/EC Reach correction command appendix XVII-552/2009/EC clause 46 (predecessor 2003/53/EC): materials or formulations with a mass concentration of NPEOs equal to or higher than 0.1% are not allowed to be put on the market when used for the following uses: industrial and institutional cleaning, household cleaning, textile and leather processing, emulsifiers for agricultural animal breast cleaning/impregnating agents, metalworking, pulp and paper manufacturing, cosmetics, other personal care products and complex excipients in pesticides and biopesticides.

While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.