CN108410413A - A kind of preparation method of paper solid gum - Google Patents
A kind of preparation method of paper solid gum Download PDFInfo
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- CN108410413A CN108410413A CN201810301313.9A CN201810301313A CN108410413A CN 108410413 A CN108410413 A CN 108410413A CN 201810301313 A CN201810301313 A CN 201810301313A CN 108410413 A CN108410413 A CN 108410413A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4266—Polycondensates having carboxylic or carbonic ester groups in the main chain prepared from hydroxycarboxylic acids and/or lactones
- C08G18/4269—Lactones
- C08G18/4277—Caprolactone and/or substituted caprolactone
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/61—Polysiloxanes
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6603—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6607—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6625—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/34
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/06—Polyurethanes from polyesters
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/08—Polyurethanes from polyethers
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Abstract
The invention discloses a kind of preparation methods of paper solid gum, belong to cultural goods field.The present invention is using isophorone diisocyanate acid esters as hard section, polycaprolactone is soft segment, introduce epoxy resin, epoxy-modified cation aqueous polyurethane emulsion is made using in-situ polymerization, paper hole is penetrated by the capillarity of Inter-fiber voids, a thin layer of film is formed in paper surface, this just makes page generate certain intensity and water repelling property, it is also carried out simultaneously using organosilicon twice-modified, it is further crosslinked and is reacted with the epoxy group of high activity by the silicone coupling agents for introducing amino-terminated, obtain the water-base polyurethane material of ternary copolymerization system, to improve the mechanical property of aqueous polyurethane film, temperature tolerance and water resistance and the surface tension for reducing film.The present invention solves at present using aqueous polyurethane emulsion as the solid gum white appearance of adhesive, and adhesive property is good, but the problem that its heat resistance, water resistance are poor.
Description
Technical field
The invention belongs to cultural goods fields, and in particular to a kind of preparation method of paper solid gum.
Background technology
Solid gum is one kind with polyvinyl alcohol（PVA）, polyvinylpyrrolidone（PVP）, acrylic resin, vinyl acetate
One or more high molecular materials such as resin are as adhesive, and fatty acid salt is as excipient, glycerine, propylene glycol, ethylene glycol etc.
For moisturizing antifreeze, water is solvent, is reacted in 70 DEG C to 90 DEG C of environment, solid adhesive obtained after filling cooling, main
It is used to paste various paper.The ph value color developing agents such as addition phenolphthalein can be made into illusion-colour solid gum, and colloid is in purple or blue, gluing
Color disappears after several seconds.Addition water-soluble dye can be made into the colour solid glue of a variety of colors, and pass through suitable modifying agent
The transparency that colloid can be adjusted, to obtain translucent or high transparency solid gum.
Presently commercially available solid gum adds the solid of moisturizer and auxiliary agent preparation using aqueous polyurethane emulsion as adhesive
Glue, the solid gum white appearance of preparation, feel is fine and smooth, and adhesive property is good, but the tolerable temperature of the solid gum is relatively low, water resistance
It is poor, easily reduce the using effect of solid gum.Therefore, prepare a kind of solid gum of higher performance needs with prodigious market
It asks.
Invention content
The technical problems to be solved by the invention：For at present using aqueous polyurethane emulsion as the solid gum appearance of adhesive
Pure white, adhesive property is good, but the problem that its heat resistance, water resistance are poor, provides a kind of preparation method of paper solid gum.
In order to solve the above technical problems, the present invention is using technical solution as described below：
A kind of preparation method of paper solid gum, the preparation method include the following steps：
（1）It counts in parts by weight, takes 10 ~ 15 parts of polycaprolactones, 5 ~ 6 parts of epoxy resin, 1 ~ 3 part of isophorone diisocyanate, 1
~ 3 parts of Isosorbide-5-Nitrae-butanediols, 0.8 ~ 1 part of dibutyl tin laurate, by polycaprolactone vacuum dehydration at 100 ~ 120 DEG C of temperature,
Under dry nitrogen protection, be cooled to 75 ~ 80 DEG C, isophorone diisocyanate be added, stand, wait for temperature be reduced to 70 ~
75 DEG C, Isosorbide-5-Nitrae-butanediol is added, dibutyl tin laurate is stood, and epoxy resin is added, keeps the temperature, must protect under temperature 70 C
Warm object；
（2）It counts in parts by weight, takes 30 ~ 40 parts of heat preservation objects, 10 ~ 15 parts of organosilicons, 3 ~ 5 parts of poly- Isopropanediols, 1 ~ 3 part of dihydroxy first
Base propionic acid, 1 ~ 3 part of N, N-dimethylformamide mix heat preservation object, organosilicon at 40 ~ 50 DEG C of temperature, and addition has
Machine silicon stands 2 ~ 3h, poly- Isopropanediol is added, and stands, is cooled to room temperature, and dihydromethyl propionic acid, N, N-dimethyl methyl is added
Amide is mixed, and is warming up to 60 DEG C, and heat preservation is cooled to room temperature, obtains cooling thing, in mass ratio 1：5 ~ 6, by cooling thing, go from
Sub- water is mixed, and 25 ~ 30min is at the uniform velocity stirred, and is adjusted pH value to 7, is obtained mixed liquor, spare；
（3）It counts in parts by weight, takes the sodium hydroxide solution, 5 ~ 7 parts of isopropanols, 2 ~ 4 parts of 3- that 10 ~ 12 parts of volume fractions are 40%
Chloro- 2- hydroxypropyls-trimethyl ammonia chloride aqueous ammonium, 1 ~ 3 part of chitosan, chitosan, sodium hydroxide solution are mixed, added
Enter isopropanol, stir lower heating water bath to 50 ~ 55 DEG C, keep the temperature 4 ~ 5h, be warming up to 60 ~ 65 DEG C, the chloro- 2- hydroxypropyls of 3--three are added
Methyl chloride aqueous ammonium stands 1 ~ 2h, adjusts pH value to 7, and filtering obtains filter cake, filter cake absolute ethyl alcohol, acetone are washed,
It is dry at 80 ~ 90 DEG C of temperature, obtain dried object；
（4）In mass ratio 1：25, dried object, water are mixed, stirred evenly, stirring liquid, in mass ratio 30 ~ 40 are obtained：3~5：1
~3：1 ~ 3, by step（2）Spare mixed liquor, stirring liquid, glycerine, excipient are put into reaction kettle, are warming up to 70 ~ 75 DEG C, are stirred
It mixes uniformly, adjusts pH value to 9, in 80 ~ 85 DEG C of heat preservations of temperature, stand defoaming, inject in mold, up to solid after cooling and shaping
Glue.
The step（2）Middle organosilicon is hydroxyl-terminated injecting two methyl siloxane.
The step（4）Middle excipient is odium stearate.
Compared with other methods, advantageous effects are the present invention：
（1）For the present invention using isophorone diisocyanate acid esters as hard section, polycaprolactone is soft segment, introduces epoxy resin, is used
Epoxy-modified cation aqueous polyurethane emulsion is made in in-situ polymerization, penetrates into paper hole by the capillarity of Inter-fiber voids
Gap forms a thin layer of film in paper surface, this just makes page generate certain intensity and water repelling property, while also using having
The progress of machine silicon is twice-modified, and the epoxy group by introducing amino-terminated silicone coupling agents and high activity is further handed over
Connection reaction, obtains the water-base polyurethane material of ternary copolymerization system, to improve mechanical property, the heatproof of aqueous polyurethane film
Property and water resistance and the surface tension for reducing film.
（2）The present invention is additionally added using 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides as modifying agent, is prepared under alkaline condition
Effect of Water Soluble Quaternary Ammonium Salt of Chitosan is mixed with aqueous polyurethane emulsion, on the one hand due to the chloro- 2- Hydroxyproyl Trimethyls chlorinations of 3-
Ammonium carries the cationic side chain unfolded, and Effect of Water Soluble Quaternary Ammonium Salt of Chitosan is positively charged, and paper is negatively charged, to further strengthen with
The addition of the adhesive property of paper, another aspect Effect of Water Soluble Quaternary Ammonium Salt of Chitosan changes the more regular close knot of aqueous polyurethane film
Crystal structure, so as to further effectively improve its water proofing property, in addition, Effect of Water Soluble Quaternary Ammonium Salt of Chitosan also has certain resist
Bacterium, antiseptic property, so as to effectively extend the quality guarantee period of solid gum, the present invention is additionally added excipient-stearic acid sodium, moisturizing
Agent-glycerine, to make solid gum that there is good plastic property and enough mechanical strengths, so that people can make its suitable when in use
Sharp ground is freely in or out with the rotation of pedestal, easy to use.
Specific implementation mode
Organosilicon is hydroxyl-terminated injecting two methyl siloxane.
Excipient is odium stearate.
A kind of preparation method of paper solid gum, the preparation method include the following steps：
（1）It counts in parts by weight, takes 10 ~ 15 parts of polycaprolactones, 5 ~ 6 parts of epoxy resin, 1 ~ 3 part of isophorone diisocyanate, 1
~ 3 parts of Isosorbide-5-Nitrae-butanediols, 0.8 ~ 1 part of dibutyl tin laurate, by polycaprolactone at 100 ~ 120 DEG C of temperature vacuum dehydration 1 ~
2h is cooled to 75 ~ 80 DEG C under dry nitrogen protection, and isophorone diisocyanate is added, and stands 1 ~ 2h, waits for that temperature drops
Down to 70 ~ 75 DEG C, Isosorbide-5-Nitrae-butanediol is added, dibutyl tin laurate stands 1 ~ 2h, epoxy resin is added, in temperature 70 C
3 ~ 4h of lower heat preservation, obtains heat preservation object；
（2）It counts in parts by weight, takes 30 ~ 40 parts of heat preservation objects, 10 ~ 15 parts of organosilicons, 3 ~ 5 parts of poly- Isopropanediols, 1 ~ 3 part of dihydroxy first
Base propionic acid, 1 ~ 3 part of N, N-dimethylformamide mix heat preservation object, organosilicon at 40 ~ 50 DEG C of temperature, and addition has
Machine silicon stands 2 ~ 3h, and poly- Isopropanediol is added, and stands 1 ~ 2h, is cooled to room temperature, and dihydromethyl propionic acid, N, N-diformazan is added
Base formamide is mixed, and is warming up to 60 DEG C, is kept the temperature 2 ~ 3h, is cooled to room temperature, obtains cooling thing, in mass ratio 1：5 ~ 6, it will cool down
Object, deionized water are mixed, and 25 ~ 30min is at the uniform velocity stirred, and are adjusted pH value to 7, are obtained mixed liquor, spare；
（3）It counts in parts by weight, takes the sodium hydroxide solution, 5 ~ 7 parts of isopropanols, 2 ~ 4 parts of 3- that 10 ~ 12 parts of volume fractions are 40%
Chloro- 2- hydroxypropyls-trimethyl ammonia chloride aqueous ammonium, 1 ~ 3 part of chitosan, chitosan, sodium hydroxide solution are mixed, added
Enter isopropanol, stir lower heating water bath to 50 ~ 55 DEG C, keep the temperature 4 ~ 5h, be warming up to 60 ~ 65 DEG C, the chloro- 2- hydroxypropyls of 3--three are added
Methyl chloride aqueous ammonium stands 1 ~ 2h, adjusts pH value to 7, and filtering obtains filter cake, filter cake absolute ethyl alcohol, acetone are washed 3 ~
It is 6 times, dry at 80 ~ 90 DEG C of temperature, obtain dried object；
（4）In mass ratio 1：25, dried object, water are mixed, stirred evenly, stirring liquid, in mass ratio 30 ~ 40 are obtained：3~5：1
~3：1 ~ 3, by step（2）Spare mixed liquor, stirring liquid, glycerine, excipient are put into reaction kettle, are warming up to 70 ~ 75 DEG C, are stirred
It mixes uniformly, adjusts pH value to 9, in 80 ~ 85 DEG C of 4 ~ 5h of heat preservation of temperature, stand defoaming, inject in mold, up to solid after cooling and shaping
Body glue.
Embodiment 1
Organosilicon is hydroxyl-terminated injecting two methyl siloxane.
Excipient is odium stearate.
A kind of preparation method of paper solid gum, the preparation method include the following steps：
（1）It counts in parts by weight, takes 10 parts of polycaprolactones, 5 parts of epoxy resin, 1 part of isophorone diisocyanate, 1 part of Isosorbide-5-Nitrae-
Butanediol, 0.8 part of dibutyl tin laurate, by polycaprolactone at 100 DEG C of temperature vacuum dehydration 1h, protected in dry nitrogen
Under shield, 75 DEG C are cooled to, isophorone diisocyanate is added, stands 1h, waits for that temperature is reduced to 70 DEG C, Isosorbide-5-Nitrae-fourth two is added
Alcohol, dibutyl tin laurate stand 1h, and epoxy resin is added, keeps the temperature 3h under temperature 70 C, obtains heat preservation object；
（2）Count in parts by weight, take 30 parts heat preservation objects, 10 parts of organosilicons, 3 parts of poly- Isopropanediols, 1 part of dihydromethyl propionic acid, 1 part
Heat preservation object, organosilicon are mixed at 40 DEG C of temperature, organosilicon are added, stands 2h, is added by N, N-dimethylformamide
Poly- Isopropanediol stands 1h, is cooled to room temperature, and dihydromethyl propionic acid, N is added, and N-dimethylformamide is mixed, and heats up
To 60 DEG C, 2h is kept the temperature, is cooled to room temperature, obtains cooling thing, in mass ratio 1：5, cooling thing, deionized water are mixed, at the uniform velocity
25min is stirred, pH value is adjusted to 7, obtains mixed liquor, it is spare；
（3）It counts in parts by weight, takes the sodium hydroxide solution, 5 parts of isopropanols, the chloro- 2- hydroxyls of 2 parts of 3- that 10 parts of volume fractions are 40%
Propyl-trimethyl ammonia chloride aqueous ammonium, 1 part of chitosan, chitosan, sodium hydroxide solution are mixed, and isopropanol is added, stirs
Lower heating water bath is mixed to 50 DEG C, keeps the temperature 4h, is warming up to 60 DEG C, the chloro- 2- hydroxypropyls-trimethyl ammonia chloride aqueous ammoniums of 3- are added, it is quiet
It sets 1h, adjusts pH value to 7, filtering obtains filter cake, filter cake absolute ethyl alcohol, acetone washs 3 times, dries, obtains at 80 DEG C of temperature
Dried object；
（4）In mass ratio 1：25, dried object, water are mixed, stirred evenly, stirring liquid, in mass ratio 30 are obtained：3：1：1, it will
Step（2）Spare mixed liquor, stirring liquid, glycerine, excipient are put into reaction kettle, are warming up to 70 DEG C, are stirred evenly, adjust pH
Value, in 80 DEG C of heat preservation 4h of temperature, stands defoaming, injects in mold, up to solid gum after cooling and shaping to 9.
Embodiment 2
Organosilicon is hydroxyl-terminated injecting two methyl siloxane.
Excipient is odium stearate.
A kind of preparation method of paper solid gum, the preparation method include the following steps：
（1）It counts in parts by weight, takes 15 parts of polycaprolactones, 6 parts of epoxy resin, 3 parts of isophorone diisocyanate, 3 parts of Isosorbide-5-Nitraes-
Butanediol, 1 part of dibutyl tin laurate, by polycaprolactone at 120 DEG C of temperature vacuum dehydration 2h, in dry nitrogen protection
Under, 80 DEG C are cooled to, isophorone diisocyanate is added, stands 2h, waits for that temperature is reduced to 75 DEG C, 1,4-butanediol is added,
Dibutyl tin laurate stands 2h, and epoxy resin is added, keeps the temperature 4h under temperature 70 C, obtains heat preservation object；
（2）Count in parts by weight, take 30 ~ 40 parts heat preservation objects, 15 parts of organosilicons, 5 parts of poly- Isopropanediols, 3 parts of dihydromethyl propionic acids,
Heat preservation object, organosilicon are mixed under temperature 50 C, organosilicon are added, stand 3h by 3 parts of N, N-dimethylformamide,
Poly- Isopropanediol is added, stands 2h, is cooled to room temperature, dihydromethyl propionic acid, N is added, N-dimethylformamide is mixed,
60 DEG C are warming up to, 3h is kept the temperature, is cooled to room temperature, obtains cooling thing, in mass ratio 1：6, cooling thing, deionized water are mixed,
30min is at the uniform velocity stirred, pH value is adjusted to 7, obtains mixed liquor, it is spare；
（3）It counts in parts by weight, takes the sodium hydroxide solution, 7 parts of isopropanols, the chloro- 2- hydroxyls of 4 parts of 3- that 12 parts of volume fractions are 40%
Propyl-trimethyl ammonia chloride aqueous ammonium, 3 parts of chitosans, chitosan, sodium hydroxide solution are mixed, and isopropanol is added, stirs
Lower heating water bath is mixed to 55 DEG C, keeps the temperature 5h, is warming up to 65 DEG C, the chloro- 2- hydroxypropyls-trimethyl ammonia chloride aqueous ammoniums of 3- are added, it is quiet
It sets 2h, adjusts pH value to 7, filtering obtains filter cake, filter cake absolute ethyl alcohol, acetone washs 6 times, dries, obtains at 90 DEG C of temperature
Dried object；
（4）In mass ratio 1：25, dried object, water are mixed, stirred evenly, stirring liquid, in mass ratio 40 are obtained：5：3：3, it will
Step（2）Spare mixed liquor, stirring liquid, glycerine, excipient are put into reaction kettle, are warming up to 75 DEG C, are stirred evenly, adjust pH
Value, in 85 DEG C of heat preservation 5h of temperature, stands defoaming, injects in mold, up to solid gum after cooling and shaping to 9.
Embodiment 3
Organosilicon is hydroxyl-terminated injecting two methyl siloxane.
Excipient is odium stearate.
A kind of preparation method of paper solid gum, the preparation method include the following steps：
（1）It counts in parts by weight, takes 13 parts of polycaprolactones, 5 parts of epoxy resin, 2 parts of isophorone diisocyanate, 2 parts of Isosorbide-5-Nitraes-
Butanediol, 0.9 part of dibutyl tin laurate, by polycaprolactone at 110 DEG C of temperature vacuum dehydration 1h, protected in dry nitrogen
Under shield, 77 DEG C are cooled to, isophorone diisocyanate is added, stands 1h, waits for that temperature is reduced to 73 DEG C, Isosorbide-5-Nitrae-fourth two is added
Alcohol, dibutyl tin laurate stand 1h, and epoxy resin is added, keeps the temperature 3h under temperature 70 C, obtains heat preservation object；
（2）Count in parts by weight, take 35 parts heat preservation objects, 13 parts of organosilicons, 4 parts of poly- Isopropanediols, 2 parts of dihydromethyl propionic acids, 2 parts
Heat preservation object, organosilicon are mixed under temperature 45 C, organosilicon are added, stand 2h, be added by N, N-dimethylformamide
Poly- Isopropanediol stands 1h, is cooled to room temperature, and dihydromethyl propionic acid, N is added, and N-dimethylformamide is mixed, and heats up
To 60 DEG C, 2h is kept the temperature, is cooled to room temperature, obtains cooling thing, in mass ratio 1：5, cooling thing, deionized water are mixed, at the uniform velocity
27min is stirred, pH value is adjusted to 7, obtains mixed liquor, it is spare；
（3）It counts in parts by weight, takes the sodium hydroxide solution, 6 parts of isopropanols, the chloro- 2- hydroxyls of 3 parts of 3- that 11 parts of volume fractions are 40%
Propyl-trimethyl ammonia chloride aqueous ammonium, 2 parts of chitosans, chitosan, sodium hydroxide solution are mixed, and isopropanol is added, stirs
Lower heating water bath is mixed to 53 DEG C, keeps the temperature 4h, is warming up to 63 DEG C, the chloro- 2- hydroxypropyls-trimethyl ammonia chloride aqueous ammoniums of 3- are added, it is quiet
It sets 1h, adjusts pH value to 7, filtering obtains filter cake, filter cake absolute ethyl alcohol, acetone washs 5 times, dries, obtains at 85 DEG C of temperature
Dried object；
（4）In mass ratio 1：25, dried object, water are mixed, stirred evenly, stirring liquid, in mass ratio 35 are obtained：4：2：2, it will
Step（2）Spare mixed liquor, stirring liquid, glycerine, excipient are put into reaction kettle, are warming up to 73 DEG C, are stirred evenly, adjust pH
Value, in 83 DEG C of heat preservation 4h of temperature, stands defoaming, injects in mold, up to solid gum after cooling and shaping to 9.
Comparative example：The solid gum of company of Ningbo City production.
The solid gum of solid gum and comparative example that embodiment is prepared respectively carries out it heat-resisting, water-fast test, surveys
Test result is shown in Table 1.
Table 1：
| Test event | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example |
| Viscosity MPas | 5423 | 5510 | 5467 | 4120~4233 |
| It impregnates in water and is placed outside rear chamber for 24 hours, crack situation | Without cracking | Without cracking | Slight cracking | Serious cracking |
| Fusing point DEG C | 204 | 211 | 206 | 152~156 |
In summary, solid adhesiveness of the invention is good, heat-resisting to be all substantially better than commercial product with water resistance performance, is worth pushing away
It is wide to use.
Claims (3)
1. a kind of preparation method of paper solid gum, which is characterized in that the preparation method includes the following steps：
（1）It counts in parts by weight, takes 10 ~ 15 parts of polycaprolactones, 5 ~ 6 parts of epoxy resin, 1 ~ 3 part of isophorone diisocyanate, 1
~ 3 parts of Isosorbide-5-Nitrae-butanediols, 0.8 ~ 1 part of dibutyl tin laurate, by polycaprolactone vacuum dehydration at 100 ~ 120 DEG C of temperature,
Under dry nitrogen protection, be cooled to 75 ~ 80 DEG C, isophorone diisocyanate be added, stand, wait for temperature be reduced to 70 ~
75 DEG C, Isosorbide-5-Nitrae-butanediol is added, dibutyl tin laurate is stood, and epoxy resin is added, keeps the temperature, must protect under temperature 70 C
Warm object；
（2）It counts in parts by weight, takes 30 ~ 40 parts of heat preservation objects, 10 ~ 15 parts of organosilicons, 3 ~ 5 parts of poly- Isopropanediols, 1 ~ 3 part of dihydroxy first
Base propionic acid, 1 ~ 3 part of N, N-dimethylformamide mix heat preservation object, organosilicon at 40 ~ 50 DEG C of temperature, and addition has
Machine silicon stands 2 ~ 3h, poly- Isopropanediol is added, and stands, is cooled to room temperature, and dihydromethyl propionic acid, N, N-dimethyl methyl is added
Amide is mixed, and is warming up to 60 DEG C, and heat preservation is cooled to room temperature, obtains cooling thing, in mass ratio 1：5 ~ 6, by cooling thing, go from
Sub- water is mixed, and 25 ~ 30min is at the uniform velocity stirred, and is adjusted pH value to 7, is obtained mixed liquor, spare；
（3）It counts in parts by weight, takes the sodium hydroxide solution, 5 ~ 7 parts of isopropanols, 2 ~ 4 parts of 3- that 10 ~ 12 parts of volume fractions are 40%
Chloro- 2- hydroxypropyls-trimethyl ammonia chloride aqueous ammonium, 1 ~ 3 part of chitosan, chitosan, sodium hydroxide solution are mixed, added
Enter isopropanol, stir lower heating water bath to 50 ~ 55 DEG C, keep the temperature 4 ~ 5h, be warming up to 60 ~ 65 DEG C, the chloro- 2- hydroxypropyls of 3--three are added
Methyl chloride aqueous ammonium stands 1 ~ 2h, adjusts pH value to 7, and filtering obtains filter cake, filter cake absolute ethyl alcohol, acetone are washed,
It is dry at 80 ~ 90 DEG C of temperature, obtain dried object；
（4）In mass ratio 1：25, dried object, water are mixed, stirred evenly, stirring liquid, in mass ratio 30 ~ 40 are obtained：3~5：1
~3：1 ~ 3, by step（2）Spare mixed liquor, stirring liquid, glycerine, excipient are put into reaction kettle, are warming up to 70 ~ 75 DEG C, are stirred
It mixes uniformly, adjusts pH value to 9, in 80 ~ 85 DEG C of heat preservations of temperature, stand defoaming, inject in mold, up to solid after cooling and shaping
Glue.
2. the preparation method of paper solid gum according to claim 1, which is characterized in that the step（2）Middle organosilicon
It is hydroxyl-terminated injecting two methyl siloxane.
3. the preparation method of paper solid gum according to claim 1, which is characterized in that the step（4）Middle excipient
It is odium stearate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810301313.9A CN108410413A (en) | 2018-04-04 | 2018-04-04 | A kind of preparation method of paper solid gum |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810301313.9A CN108410413A (en) | 2018-04-04 | 2018-04-04 | A kind of preparation method of paper solid gum |
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ID=63134674
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| CN201810301313.9A Withdrawn CN108410413A (en) | 2018-04-04 | 2018-04-04 | A kind of preparation method of paper solid gum |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112426890A (en) * | 2020-12-01 | 2021-03-02 | 赖枝帅 | Anti-pollution modified polyvinyl chloride composite membrane and preparation method thereof |
-
2018
- 2018-04-04 CN CN201810301313.9A patent/CN108410413A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112426890A (en) * | 2020-12-01 | 2021-03-02 | 赖枝帅 | Anti-pollution modified polyvinyl chloride composite membrane and preparation method thereof |
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