1. A pathological specimen sealing liquid is characterized in that: the raw materials of the pathological specimen sealing liquid comprise an oligomer, an active monomer, an initiator, a flatting agent, a defoaming agent, a coupling agent and an antioxidant; the parts of the raw materials are 30-55 parts of oligomer, 45-60 parts of active monomer, 3-10 parts of initiator, 0.1-1 part of flatting agent, 0.1-1 part of defoaming agent, 0.1-1 part of coupling agent and 0.1-1 part of antioxidant.

2. The pathological specimen sealing liquid according to claim 1, wherein: the oligomer is one or a mixture of polyester acrylic resin, polyurethane acrylic resin, epoxy modified acrylic resin and acrylic resin.

3. The pathological specimen sealing liquid according to claim 2, wherein: the polyurethane acrylic resin is aliphatic polyurethane acrylic resin, and the epoxy modified acrylic resin is bisphenol A epoxy acrylic resin.

4. The pathological specimen sealing liquid according to claim 3, wherein: the active monomer is one or a mixture of more of isobornyl acrylate, isobornyl methacrylate, hydroxyethyl methacrylate, 1, 6-hexanediol diacrylate, tripropylene glycol diacrylate, neopentyl glycol diacrylate, trimethylolpropane triacrylate, pentaerythritol triacrylate and dipentaerythritol hexaacrylate.

5. The pathological specimen sealing liquid according to claim 4, wherein: the initiator is one or a mixture of 2-hydroxy-2-methyl-1-phenyl acetone, 1-hydroxycyclohexyl phenyl ketone, 2,4, 6-trimethyl benzoyl diphenyl phosphine oxide, 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-acetone, phenyl bis (2,4, 6-trimethyl benzoyl) phosphine oxide, benzophenone, 2-isopropyl thioxanthone, 2, 4-diethyl thioxanthone and organic amine.

6. The pathological specimen sealing liquid according to claim 5, wherein: the leveling agent is one or a mixture of BYK333 and TEGO 2100; the antifoaming agent is one or a mixture of TEGO920 and KS 66; the coupling agent is one or a mixture of KH550, KH560 and KH 570; the antioxidant is one or more of antioxidant 6026, antioxidant 1010 and antioxidant 1076.

7. The method for preparing the pathological specimen sealing liquid according to claim 6, wherein the method comprises the following steps: the method comprises the following steps:

s1, weighing the oligomer, the active monomer, the initiator, the leveling agent, the defoaming agent, the coupling agent and the antioxidant according to parts;

s2, sequentially adding the oligomer, the active monomer, the initiator, the flatting agent, the defoaming agent, the coupling agent and the antioxidant into a container to obtain a mixed solution;

s3, keeping the temperature in the container at 40-55 ℃, stirring for 10-20 minutes at the rotating speed of 1000-2000 rpm/min by using a stirrer, and then slowly stirring at a reduced rotating speed until bubbles in the mixed solution in the container are gradually eliminated;

and S4, filtering the mixed solution by using a filter screen, then performing air suction and defoaming treatment on the filtrate by using a vacuum air pump, and standing and cooling the filtrate to obtain the prepared pathological specimen sealing liquid.

8. The method for preparing the pathological specimen sealing liquid according to claim 7, wherein the method comprises the following steps: the filter screen in the step S4 is a 1000-mesh filter screen.

9. The method for sealing the pathological specimen according to claim 6, comprising: the method comprises the following steps:

placing a processed specimen glass slide in a horizontal position, and then coating a pathological specimen sealing liquid on the surface of the glass slide;

and step two, after the pathological specimen sealing liquid is leveled on the surface of the glass slide, irradiating the pathological specimen sealing liquid by using ultraviolet light to complete the sealing operation of the specimen glass slide.

10. The method for sealing a pathological specimen sealing liquid according to claim 9, comprising: in the second step, the wavelength of the ultraviolet light is 365-405 nm, and the illumination intensity is 60-300 mW/cm²The illumination time is 5-60 s.

Background

The current common specimen is in the form of a glass slide, an adhesive and a cover glass, and the manufacturing method comprises two methods, namely manual and mechanical.

The manual method has the following disadvantages: the cover glass is very thin, and is easy to cut and leave fingerprints when being held by hands, so that the observation under a microscope is influenced; when the forceps are used for clamping, the clamping is easy to crack or break; meanwhile, the requirement of manual sealing on operators is high, the quantity of the adhesive (glue) required by each sheet needs to be controlled, and glue leakage and glue overflow cannot occur; the operation method is required, and the generation of bubbles is avoided; in addition, the covering pressure is controlled, so that the sample cannot be damaged and the observation cannot be influenced.

Machine film sealing is commonly used in hospital pathology department, and full-automatic dyeing film sealing machine is adopted. Although the film sealing machine has promoted work efficiency greatly for the section quality is more normal and standardized, its film sealing is with high costs, consume fast, will cooperate solvent xylol to use when the film sealing simultaneously, and xylol is poisonous and have pungent smell, and long-term use can influence operating personnel's health. In addition, in clinical practice, the specimens sealed and stored by the film have fading phenomena after years, which affect the needs of the return visit or scientific research and can not meet the medical use requirements.

Disclosure of Invention

The invention aims to solve the problems and provides a pathological specimen sealing liquid with higher sealing efficiency and better using effect, and a preparation method and a sealing method thereof.

In order to achieve the purpose, the technical scheme of the invention is as follows:

the pathological specimen sealing liquid comprises raw materials of oligomer, active monomer, initiator, flatting agent, defoaming agent, coupling agent and antioxidant; the parts of the raw materials are 30-55 parts of oligomer, 45-60 parts of active monomer, 3-10 parts of initiator, 0.1-1 part of flatting agent, 0.1-1 part of defoaming agent, 0.1-1 part of coupling agent and 0.1-1 part of antioxidant.

Further, the oligomer is one or a mixture of polyester acrylic resin, polyurethane acrylic resin, epoxy modified acrylic resin and acrylic resin.

Further, the polyurethane acrylic resin is aliphatic polyurethane acrylic resin, and the epoxy modified acrylic resin is bisphenol A epoxy acrylic resin.

Further, the active monomer is one or a mixture of more of isobornyl acrylate, isobornyl methacrylate, hydroxyethyl methacrylate, 1, 6-hexanediol diacrylate, tripropylene glycol diacrylate, neopentyl glycol diacrylate, trimethylolpropane triacrylate, pentaerythritol triacrylate and dipentaerythritol hexaacrylate.

Further, the initiator is one or a mixture of more of 2-hydroxy-2-methyl-1-phenyl acetone, 1-hydroxycyclohexyl phenyl ketone, 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide, 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-acetone, phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide, benzophenone, 2-isopropyl thioxanthone, 2, 4-diethyl thioxanthone and organic amine.

Further, the leveling agent is one or a mixture of BYK333 and TEGO 2100; the antifoaming agent is one or a mixture of TEGO920 and KS 66; the coupling agent is one or a mixture of KH550, KH560 and KH 570; the antioxidant is one or more of antioxidant 6026, antioxidant 1010 and antioxidant 1076.

A preparation method of a pathological specimen sealing liquid comprises the following steps:

s1, weighing the oligomer, the active monomer, the initiator, the leveling agent, the defoaming agent, the coupling agent and the antioxidant according to parts;

s2, sequentially adding the oligomer, the active monomer, the initiator, the flatting agent, the defoaming agent, the coupling agent and the antioxidant into a container to obtain a mixed solution;

s3, keeping the temperature in the container at 40-55 ℃, stirring for 10-20 minutes at the rotating speed of 1000-2000 rpm/min by using a stirrer, and then slowly stirring at a reduced rotating speed until bubbles in the mixed solution in the container are gradually eliminated;

and S4, filtering the mixed solution by using a filter screen, then performing air suction and defoaming treatment on the filtrate by using a vacuum air pump, and standing and cooling the filtrate to obtain the prepared pathological specimen sealing liquid.

Further, the filter screen in the step S4 is a 1000-mesh filter screen.

A method for sealing and fixing a pathological specimen sealing liquid comprises the following steps:

placing a processed specimen glass slide in a horizontal position, and then coating a pathological specimen sealing liquid on the surface of the glass slide;

and step two, after the pathological specimen sealing liquid is leveled on the surface of the glass slide, irradiating the pathological specimen sealing liquid by using ultraviolet light to complete the sealing operation of the specimen glass slide.

Further, in the second step, the wavelength of the ultraviolet light is 365-405 nm, and the illumination intensity is 60-300 mW/cm²The illumination time is 5-60 s.

Compared with the prior art, the invention has the advantages and positive effects that:

1. the pathological specimen sealing liquid has the advantages of strong adhesion, quick drying, good hardness, scratch resistance, high transparency, good weather resistance, no bubbles, high light transmittance and the like, can be cured after being irradiated by ultraviolet light, has a flat surface after being sealed, is fog-free, yellowing-resistant and crack-free, and can completely replace a cover glass;

2. the initiator contained in the invention generates active free radicals or cations after absorbing ultraviolet light, thereby initiating monomer polymerization and crosslinking chemical reaction, converting the liquid state of the pathological specimen sealing liquid into a solid state within seconds, and improving the sealing efficiency of the glass slide;

3. the pathological specimen sealing liquid has no VOC volatile matter, all components of the pathological specimen sealing liquid are not limited in environmental regulations, the pathological specimen sealing liquid has a good environmental protection effect, the curing speed is high, the curing can be finished within several seconds to dozens of seconds, and the detection and carrying operation can be carried out after the curing, so that the pathological specimen sealing liquid is beneficial to automatic production and can obviously improve the production rate;

4. the antioxidant contained in the invention is helpful for delaying the aging and yellowing of the specimen slice, so that the specimen slice can still keep better color after years, the storage time of the sample is prolonged, and the medical use requirement can be met.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.

FIG. 1 is a diagram illustrating the effect of the present invention.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived from the embodiments of the present invention by a person skilled in the art without any creative effort, should be included in the protection scope of the present invention.

Example 1

1) 45 parts of polyester acrylic resin, 5 parts of isobornyl methacrylate, 20 parts of 1, 6-hexanediol diacrylate, 15 parts of tripropylene glycol diacrylate, 10 parts of dipentaerythritol hexaacrylate, 2 parts of 1-hydroxycyclohexyl phenyl ketone, 2 parts of 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide, 0.5 part of a leveling agent BYK333, 0.5 part of an antifoaming agent TEGO920, 1 part of a coupling agent KH550 and 0.5 part of an antioxidant 6026 are used for preparing the pathological specimen sealing liquid.

2) And placing the pretreated specimen glass slide in a horizontal position, coating the pathological specimen sealing liquid, quickly leveling, and irradiating by ultraviolet light to obtain the pathological specimen sealing liquid-sealed glass slide.

3) The obtained pathological specimen sealing liquid has smooth and flat sealing coating and overall light transmittance of more than 90 percent. The hardness of the coating is tested by a pencil hardness tester, and reaches H grade by a Chinese drawing pencil and 750g force. The adhesion of the coating was tested with a cross-cut tape and found to be grade 1.

Example 2

1) 50 parts of polyurethane acrylic resin, 5 parts of isobornyl acrylate, 15 parts of tripropylene glycol diacrylate, 10 parts of trimethylolpropane triacrylate, 10 parts of pentaerythritol triacrylate, 3 parts of 2-hydroxy-2-methyl-1-phenyl acetone, 1 part of phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide, 0.5 part of a flatting agent BYK333, 0.5 part of a defoaming agent TEGO920, 1 part of a coupling agent KH560 and 0.5 part of an antioxidant 1010 are used for preparing the pathological specimen sealing liquid.

2) And placing the pretreated specimen glass slide in a horizontal position, coating the pathological specimen sealing liquid, quickly leveling, and irradiating by ultraviolet light to obtain the pathological specimen sealing liquid-sealed glass slide.

3) The obtained pathological specimen sealing liquid has smooth and flat sealing coating and overall light transmittance of more than 90 percent. The hardness of the coating is tested by a pencil hardness tester, and reaches H grade by a Chinese drawing pencil and 750g force. The adhesion of the coating was tested with a cross-cut tape and found to be grade 1.

Example 3

1) 55 parts of epoxy modified acrylic resin, 8 parts of hydroxyethyl methacrylate, 10 parts of neopentyl glycol diacrylate, 12 parts of trimethylolpropane triacrylate, 10 parts of dipentaerythritol hexaacrylate, 3 parts of 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-acetone, 2 parts of 2-isopropyl thioxanthone, 0.4 part of a flatting agent TEGO2100, 0.3 part of an antifoaming agent KS66, 1 part of a coupling agent KH570 and 0.5 part of an antioxidant 6026 are used for preparing the pathological specimen sealing liquid.

2) And placing the pretreated specimen glass slide in a horizontal position, coating the pathological specimen sealing liquid, quickly leveling, and irradiating by ultraviolet light to obtain the pathological specimen sealing liquid-sealed glass slide.

3) The obtained pathological specimen sealing liquid has smooth and flat sealing coating, and the whole light transmittance reaches more than 91 percent. The hardness of the coating is tested by a pencil hardness tester, and reaches H grade by a Chinese drawing pencil and 750g force. The adhesion of the coating was tested with a cross-cut tape and found to be grade 1.

Example 4

1) 20 parts of polyester acrylic resin, 25 parts of epoxy modified acrylic resin, 5 parts of isobornyl methacrylate, 20 parts of neopentyl glycol diacrylate, 25 parts of pentaerythritol triacrylate, 5 parts of organic amine, 2 parts of benzophenone, 2 parts of 1-hydroxycyclohexyl phenyl ketone, 1 part of 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, 0.4 part of a flatting agent BYK333, 0.5 part of a defoaming agent TEGO920, 1 part of a coupling agent KH550 and 0.5 part of an antioxidant 1076 are used for preparing the pathological specimen sealing liquid.

2) And placing the pretreated specimen glass slide in a horizontal position, coating the pathological specimen sealing liquid, quickly leveling, and irradiating by ultraviolet light to obtain the pathological specimen sealing liquid-sealed glass slide.

3) The obtained pathological specimen sealing liquid has smooth and flat sealing coating and overall light transmittance of more than 90 percent. The hardness of the coating is tested by a pencil hardness tester, and reaches H grade by a Chinese drawing pencil and 750g force. The adhesion of the coating was tested with a cross-cut tape and found to be grade 1.

Example 5

1) The pathological specimen sealing liquid is prepared from 20 parts of polyurethane acrylic resin, 30 parts of epoxy modified acrylic resin, 5 parts of isobornyl acrylate, 15 parts of 1, 6-hexanediol diacrylate, 15 parts of trimethylolpropane triacrylate, 10 parts of dipentaerythritol hexaacrylate, 4 parts of organic amine, 1.5 parts of benzophenone, 3 parts of 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-acetone, 1 part of 2-isopropyl thioxanthone, 0.3 part of flatting agent TEGO2100, 0.5 part of defoaming agent KS66, 1 part of coupling agent KH570 and 0.5 part of antioxidant 6026.

2) And placing the pretreated specimen glass slide in a horizontal position, coating the pathological specimen sealing liquid, quickly leveling, and irradiating by ultraviolet light to obtain the pathological specimen sealing liquid-sealed glass slide.

3) The obtained pathological specimen sealing liquid has smooth and flat sealing coating and overall light transmittance of more than 90 percent. The hardness of the coating is tested by a pencil hardness tester, and reaches H grade by a Chinese drawing pencil and 750g force. The adhesion of the coating was tested with a cross-cut tape and found to be grade 1.

Example 6

1) The pathological specimen sealing liquid is prepared from 35 parts of epoxy modified acrylic resin, 20 parts of acrylic resin, 5 parts of hydroxyethyl methacrylate, 20 parts of neopentyl glycol diacrylate, 10 parts of pentaerythritol triacrylate, 5 parts of dipentaerythritol hexaacrylate, 4.5 parts of organic amine, 1 part of benzophenone, 3 parts of 2-hydroxy-2-methyl-1-phenyl acetone, 1 part of 2, 4-diethyl thioxanthone, 0.5 part of flatting agent BYK333, 0.4 part of defoaming agent TEGO920, 1 part of coupling agent KH560 and 0.5 part of antioxidant 6026.

2) And placing the pretreated specimen glass slide in a horizontal position, coating the pathological specimen sealing liquid, quickly leveling, and irradiating by ultraviolet light to obtain the pathological specimen sealing liquid-sealed glass slide.

3) The obtained pathological specimen sealing liquid has smooth and flat sealing coating and overall light transmittance of more than 90 percent. The hardness of the coating is tested by a pencil hardness tester, and reaches H grade by a Chinese drawing pencil and 750g force. The adhesion of the coating was tested with a cross-cut tape and found to be grade 1.

Example 7

1) 28 parts of polyester acrylic resin, 22 parts of acrylic resin, 20 parts of 1, 6-hexanediol diacrylate, 20 parts of trimethylolpropane triacrylate, 5 parts of dipentaerythritol hexaacrylate, 1 part of benzophenone, 4 parts of 1-hydroxycyclohexyl phenyl ketone, 1 part of 2, 4-diethyl thioxanthone, 0.4 part of a leveling agent BYK333, 0.5 part of an antifoaming agent KS66, 1 part of a coupling agent KH550 and 0.5 part of an antioxidant 6026 are used for preparing the pathological specimen sealing liquid.

2) And placing the pretreated specimen glass slide in a horizontal position, coating the pathological specimen sealing liquid, quickly leveling, and irradiating by ultraviolet light to obtain the pathological specimen sealing liquid-sealed glass slide.

3) The obtained pathological specimen sealing liquid has smooth and flat sealing coating and overall light transmittance of more than 90 percent. The hardness of the coating is tested by a pencil hardness tester, and reaches H grade by a Chinese drawing pencil and 750g force. The adhesion of the coating was tested with a cross-cut tape and found to be grade 1.

Example 8

1) The pathological specimen sealing liquid is prepared from 30 parts of polyurethane acrylic resin, 18 parts of acrylic resin, 22 parts of neopentyl glycol diacrylate, 15 parts of trimethylolpropane triacrylate, 10 parts of pentaerythritol triacrylate, 2 parts of 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, 3 parts of 1-hydroxycyclohexyl phenyl ketone, 1 part of 2-isopropyl thioxanthone, 0.5 part of a leveling agent TEGO2100, 0.5 part of a defoaming agent TEGO920, 1 part of a coupling agent KH570 and 0.5 part of an antioxidant 1010.

2) And placing the pretreated specimen glass slide in a horizontal position, coating the pathological specimen sealing liquid, quickly leveling, and irradiating by ultraviolet light to obtain the pathological specimen sealing liquid-sealed glass slide.

3) The obtained pathological specimen sealing liquid has smooth and flat sealing coating and overall light transmittance of more than 90 percent. The hardness of the coating is tested by a pencil hardness tester, and reaches H grade by a Chinese drawing pencil and 750g force. The adhesion of the coating was tested with a cross-cut tape and found to be grade 1.

Example 9

1) The pathological specimen sealing liquid is prepared from 32 parts of polyester acrylic resin, 20 parts of polyurethane acrylic resin, 5 parts of hydroxyethyl methacrylate, 30 parts of pentaerythritol triacrylate, 8 parts of dipentaerythritol hexaacrylate, 1 part of 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, 3 parts of 2-hydroxy-2-methyl-1-phenyl acetone, 1 part of 2, 4-diethylthioxanthone, 0.5 part of a flatting agent BYK333, 0.5 part of a defoaming agent TEGO920, 1 part of a coupling agent KH550 and 0.5 part of an antioxidant 6026.

2) And placing the pretreated specimen glass slide in a horizontal position, coating the pathological specimen sealing liquid, quickly leveling, and irradiating by ultraviolet light to obtain the pathological specimen sealing liquid-sealed glass slide.

3) The obtained pathological specimen sealing liquid has smooth and flat sealing coating and overall light transmittance of more than 90 percent. The hardness of the coating is tested by a pencil hardness tester, and reaches H grade by a Chinese drawing pencil and 750g force. The adhesion of the coating was tested with a cross-cut tape and found to be grade 1.

Example 10

1) The pathological specimen sealing liquid is prepared from 10 parts of polyester acrylic resin, 12 parts of polyurethane acrylic resin, 18 parts of epoxy modified acrylic resin, 5 parts of hydroxyethyl methacrylate, 20 parts of tripropylene glycol diacrylate, 30 parts of pentaerythritol triacrylate, 1 part of phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide, 4 parts of 2-hydroxy-2-methyl-1-phenyl acetone, 0.5 part of a flatting agent BYK333, 0.5 part of a defoaming agent TEGO920, 1 part of a coupling agent KH560 and 0.5 part of an antioxidant 6026.

2) And placing the pretreated specimen glass slide in a horizontal position, coating the pathological specimen sealing liquid, quickly leveling, and irradiating by ultraviolet light to obtain the pathological specimen sealing liquid-sealed glass slide.

3) The obtained pathological specimen sealing liquid has smooth and flat sealing coating and overall light transmittance of more than 90 percent. The hardness of the coating is tested by a pencil hardness tester, and reaches H grade by a Chinese drawing pencil and 750g force. The adhesion of the coating was tested with a cross-cut tape and found to be grade 1.

As shown in figure 1, when the invention is used, firstly a specimen 2 is placed on a glass slide 1, then a pathological specimen sealing liquid is coated on the specimen 2 and the glass slide 1, and a sealing coating 3 is formed after ultraviolet irradiation, so that the use effect is better, and the pathological specimen sealing liquid in the invention can completely replace a cover glass.

After the specimen and the glass slide are processed, directly coating the pathological specimen sealing liquid after vacuumizing on a cell or tissue specimen, clarifying and brightening the specimen without generating bubbles basically, leveling for 5-10 s, and then performing light intensity of 60-300 mW/cm at a wavelength of 365-405 nm and light intensity of 365-300 mW/cm²The ultraviolet light irradiates for about 5-60 s, is basically and completely sealed, has no shrinkage deformation, is safe, simple and convenient to operate and has low cost; and the pathological specimen sealing liquid can be coated by a dispenser to realize accurate operation, the thickness of the adhesive layer can be adjusted within the range of 50-250 um according to the requirement, and the using effect of the invention is further improved.

The invention has the following beneficial effects:

1. the pathological specimen sealing liquid has the advantages of strong adhesion, quick drying, good hardness, scratch resistance, high transparency, good weather resistance, no bubbles, high light transmittance and the like, can be cured after being irradiated by ultraviolet light, has a flat surface after being sealed, is fog-free, yellowing-resistant and crack-free, and can completely replace a cover glass;

2. the initiator contained in the invention generates active free radicals or cations after absorbing ultraviolet light, thereby initiating monomer polymerization and crosslinking chemical reaction, converting the liquid state of the pathological specimen sealing liquid into a solid state within seconds, and improving the sealing efficiency of the glass slide;

3. the pathological specimen sealing liquid has no VOC volatile matter, all components of the pathological specimen sealing liquid are not limited in environmental regulations, the pathological specimen sealing liquid has a good environmental protection effect, the curing speed is high, the curing can be finished within several seconds to dozens of seconds, and the detection and carrying operation can be carried out after the curing, so that the pathological specimen sealing liquid is beneficial to automatic production and can obviously improve the production rate;

4. the antioxidant contained in the invention is helpful for delaying the aging and yellowing of the specimen slice, so that the specimen slice can still keep better color after years, the storage time of the sample is prolonged, and the medical use requirement can be met.