CN106497470A - A kind of preparation method of high viscosity aging resistance casting glue - Google Patents
A kind of preparation method of high viscosity aging resistance casting glue Download PDFInfo
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- CN106497470A CN106497470A CN201610946918.4A CN201610946918A CN106497470A CN 106497470 A CN106497470 A CN 106497470A CN 201610946918 A CN201610946918 A CN 201610946918A CN 106497470 A CN106497470 A CN 106497470A
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- C—CHEMISTRY; METALLURGY
- 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
- C09J161/00—Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
- C09J161/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C09J161/32—Modified amine-aldehyde condensates
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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
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/40—Chemically modified polycondensates
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- C—CHEMISTRY; METALLURGY
- 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
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- 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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The present invention relates to a kind of preparation method of high viscosity aging resistance casting glue, belongs to casting glue preparing technical field.The present invention is beaten first with taking Fructus Hordei Germinatus, digested with multiple, after enzymolysis, enzyme denaturing obtains maltose syrup, by maltose syrup, reacted under high temperature and alkalescence condition using maltose syrup, formalin and tripolycyanamide, the glue of high viscosity can be obtained after reaction, it is that catalyst and vinyl-terminated silicone fluid are prepared into component A by the glue of high viscosity, platinum dioxide, vinyl-terminated silicone fluid, containing hydrogen silicone oil are prepared component B again, by component A and the dirty vacuum defoamation of component B mixing, you can obtain high viscosity aging resistance casting glue.High viscosity aging resistance casting glue viscosity coefficient prepared by the present invention is high, improves the cohesive with base material, and difficult for drop-off, embedding effect is good, and the growth with use time, is difficult to turn to be yellow, and ageing resistace is good.
Description
Technical field
The present invention relates to a kind of preparation method of high viscosity aging resistance casting glue, belongs to casting glue preparing technical field.
Background technology
The noun of casting glue or fluid sealant has play an indispensable role in the modern life, be applied to window frame,
Doorframe, skirting, edging, skylight, tank, air vent, bridge fill up maintenance, building structure curtain wall and joint filling, the caulking joint of pipeline
In sealing, general casting glue need to be generally chronically exposed in the environment of air and different temperatures, therefore needed with weatherability, prevented
The function such as water and obstruct aqueous vapor, if in the environment of being further chronically exposed to ultraviolet radiation, then can add additive to make which
There is anti-ultraviolet function.Casting glue also apply be applicable to LED application materials, chip package, solar cell application material, its
The protective coating of his electronics or electrical industry, mould material etc., can be also widely applied to automotive electronic industry and domestic electronic appliances
In field.
Embedding Material mainly has epoxy resin, organosilicon and polyurethane three major types at present：Wherein epoxy resin casting glue
Low price, adhesive property are excellent, electrical insulating property is good, but low temperature flexibility is poor, weatherability is poor, shrinkage factor is big；Silicone embedding
Glue good flame resistance, resistant of high or low temperature are excellent, but price height, electrical insulating property are poor；Polyurethaness casting glue combines epoxy resin
With the advantage of silicone casting glue, and soft durometer, curing rate can be adjusted by formula, with excellent damping, water-fast, resistance to
Mill and the performance such as low temperature resistant, are widely used in embedding field.
In a kind of polyurethane pouring sealant being made up of component A and B component of existing patent, wherein, diluent-fatty acid methyl ester
Or dioctyl phthalate, two fourth stannum of catalyst-lauric acid or stannous octoate；Component A is：60～80 weight portion terminal hydroxy groups gather
Butadiene, 10～25 parts by weight diluent, 5～15 weight portion white carbons；B component is：80～95 weight portions liquefaction diphenylmethyl
Alkane diisocyanate, 5～20 part by weight of catalyst.By component A and B component according to 1 during use:1～1.5 ratio mix homogeneously
After pour into a mould.The method technique is relatively simple, and performance can reach the performance that " pre-polymerization method " prepares product, but is often carrying out embedding
During glue caulking joint, because curing reaction causes casting glue, surface energy is low, and very poor with the cohesive of base material, improves when viscosifier are added
During the cohesive of casting glue and base material, can cause again to seal and the effect of caulking joint is bad, or insufficient strength causes somewhat to touch
Will result in at sealing and come off, while long-time is exposed under wet gas environments or light irradiation so that casting glue produces xanthochromia
And causing sealing and the effect of caulking joint to decline, ageing resistace is not good.
Content of the invention
The technical problem to be solved：It is poor with the adhesive property of base material for existing polyurethane pouring sealant,
Intensity is not high, easy to fall off, causes embedding effect bad, and the not good problem of ageing resistace, the invention provides a kind of utilize
Maltose syrup, formalin and tripolycyanamide are prepared into high-viscosity glue, can prepare high viscosity with vinyl-terminated silicone fluid and resist
The method of aging casting glue, the present invention are beaten first with taking Fructus Hordei Germinatus, are digested with multiple, and after enzymolysis, enzyme denaturing obtains maltose
Slurry, maltose syrup is reacted under high temperature and alkalescence condition using maltose syrup, formalin and tripolycyanamide, is reacted
The glue of high viscosity can be obtained afterwards, be that catalyst and vinyl-terminated silicone fluid are prepared into group by the glue of high viscosity, platinum dioxide
Divide A, then vinyl-terminated silicone fluid, containing hydrogen silicone oil are prepared component B, by component A and the dirty vacuum defoamation of component B mixing, you can obtain high
Viscosity aging resistance casting glue.High viscosity aging resistance casting glue viscosity coefficient prepared by the present invention is high, improves the bonding with base material
Property, difficult for drop-off, embedding effect is good, and the growth with use time, is difficult to turn to be yellow, and ageing resistace is good.
For solving above-mentioned technical problem, the technical solution used in the present invention is：
（1）Weigh 200～300g Fructus Hordei Germinatus, be placed in beater after peeling, and add 100～200g deionized waters, beating 30～
With 3 layers of filtered through gauze after 40min, filtering residue is collected, filtering residue is put in baking oven, at 60～70 DEG C, dry 6～8h, after drying
Filtering residue add super micron mill in crush, cross 150～170 mesh sieves, obtain powder；
（2）By above-mentioned powder in mass ratio 1:5 are mixed with pH6.5 NaAc_HAc buffer solutions, stirring 20～30min of mixing
Obtain suspension afterwards, 0.3～0.5g enzymatic activity 100～200u/g Thermostable α-Amylases are added in suspension, after stirring mixing
Be warming up to 90～95 DEG C, insulation enzymolysis 3～5h, after enzymolysis at a temperature of 140～160 DEG C 4～6h of enzyme denaturing, be cooled to 50 after enzyme denaturing
～55 DEG C, and be 5.0～5.5 with 15% salt acid for adjusting pH value of mass fraction, 0.3～0.5g enzymatic activitys 100 are sequentially added after regulation
～200u/g beta amylases and 0.1～0.3g enzymatic activity 10～20u/g pullulanase, stirring 2～3h of mixing, 200 after stirring
10～15min of enzyme denaturing at a temperature of～220 DEG C, filters after enzyme denaturing, collects filtrate,
（3）Measure 80～100mL mass fractions, 5% formalin to add in there-necked flask, molten with 15% sodium hydroxide of mass fraction
Liquid adjust pH value be 9.0～10.0, there-necked flask is put in oil bath pan, 70～80 DEG C are heated to, insulated and stirred mixing 5～
0.5～0.7g Boraxs are added after 10min, add 30～50g tripolycyanamide and the above-mentioned filtrates of 60～80g, with 2 to Borax dissolving
～3 DEG C/min ramps to 90～100 DEG C, 2～3h of insulated and stirred, adjusting pH value with 5% sodium hydroxide solution of mass fraction is
9.0～10.0, room temperature is cooled to after regulation, obtain dope；
（4）60～80g above-mentioned dope, 0.1～0.2g platinum dioxide, 0.08～0.10g vinyl-terminated silicone fluid are weighed respectively,
Under 800～1000r/min rotating speeds, 25～30min of stirring mixing, obtains component A；
（5）Weigh 60～80g vinyl-terminated silicone fluids, 6～8g containing hydrogen silicone oils respectively, stir under 800～1000r/min rotating speeds mixed
25～30min is closed, component B is obtained, by component A and component B in mass ratio 1 of above-mentioned preparation:1 mixing, is turned with 600～800r/min
3～5min of vacuum defoamation after speed 20～30min of mixing, you can obtain high viscosity aging resistance casting glue.
The application process of the present invention：High viscosity aging resistance embedding prepared by the present invention is injected first in LED shaping mold cavities
Glue, after the completion of the good LED support that is inserted into pressure welding is inserted into, is put in baking oven and is solidified, and the temperature controlled in baking oven is
120～135 DEG C, after 45～60min of solidification, LED is deviate from from die cavity.After testing, the high viscosity that prepared by the present invention resists
Aging embedding adhesiveness reaches 5000～8500mPa s, and heat conductivity reaches 1.7～2.5W/m k, and hardness reaches 65～
70H, tensile strength reach 3.7～4.5MPa.
Compared with additive method, Advantageous Effects are the present invention：
（1）High viscosity aging resistance casting glue prepared by the present invention is preferable with the cohesive of base material, and difficult for drop-off, viscosity reaches 5000
～8500mPa s；
（2）High viscosity aging resistance casting glue prepared by the present invention is difficult to turn to be yellow with the growth of use time, ageing resistace
Good；
（3）Preparation process of the present invention is simple, and raw material is obtained simply, and cost is relatively low.
Specific embodiment
Weigh 200～300g Fructus Hordei Germinatus first, be placed in beater after peeling, and add 100～200g deionized waters, be beaten
With 3 layers of filtered through gauze after 30～40min, filtering residue is collected, filtering residue is put in baking oven, at 60～70 DEG C, dry 6～8h, will be dry
Filtering residue after dry is added in super micron mill and is crushed, and is crossed 150～170 mesh sieves, is obtained powder；By above-mentioned powder in mass ratio 1:5 with
PH6.5 NaAc_HAc buffer solutions mix, stirring mixing 20～30min after suspension, in suspension add 0.3～
0.5g enzymatic activity 100～200u/g Thermostable α-Amylases, are warming up to 90～95 DEG C after stirring mixing, insulation 3～5h of enzymolysis, enzyme
After solution at a temperature of 140～160 DEG C 4～6h of enzyme denaturing, be cooled to 50～55 DEG C after enzyme denaturing, and with 15% hydrochloric acid of mass fraction adjust
PH value is 5.0～5.5, sequentially adds 0.3～0.5g, 100～200u/g of enzymatic activity beta amylases and 0.1～0.3g enzymes after regulation
Activity 10～20u/g pullulanase, stirring mixing 2～3h, after stirring at a temperature of 200～220 DEG C 10～15min of enzyme denaturing, go out
Filter after enzyme, collect filtrate, measure 80～100mL mass fractions, 5% formalin and add in there-necked flask, with mass fraction 15%
It is 9.0～10.0 that sodium hydroxide solution adjusts pH value, and there-necked flask is put in oil bath pan, 70～80 DEG C are heated to, and insulation is stirred
0.5～0.7g Boraxs are added after mixing 5～10min of mixing, is added on 30～50g tripolycyanamide and 60～80g to Borax dissolving
Filtrate is stated, with 2～3 DEG C/min ramps to 90～100 DEG C, 2～3h of insulated and stirred, with 5% sodium hydroxide solution of mass fraction
It is 9.0～10.0 to adjust pH value, is cooled to room temperature, obtains dope after regulation；Weigh respectively the above-mentioned dopes of 60～80g, 0.1～
0.2g platinum dioxides, 0.08～0.10g vinyl-terminated silicone fluids, 25～30min of stirring mixing under 800～1000r/min rotating speeds,
Obtain component A；60～80g vinyl-terminated silicone fluid, 6～8g containing hydrogen silicone oil are finally weighed respectively, under 800～1000r/min rotating speeds
Stirring 25～30min of mixing, obtains component B, by component A and component B in mass ratio 1 of above-mentioned preparation:1 mixing, with 600～
800r/min rotating speeds mix 3～5min of vacuum defoamation after 20～30min, you can obtain high viscosity aging resistance casting glue.
Example 1
Weigh 300g Fructus Hordei Germinatus first, be placed in beater after peeling, and add 200g deionized waters, with 3 layers of yarn after beating 40min
Cloth is filtered, and collects filtering residue, filtering residue is put in baking oven, 8h is dried at 70 DEG C, and dried filtering residue is added super micron mill
Middle crushing, crosses 170 mesh sieves, obtains powder；By above-mentioned powder in mass ratio 1:5 are mixed with pH6.5 NaAc_HAc buffer solutions,
Suspension is obtained after stirring mixing 30min, and 0.5g enzymatic activity 200u/g Thermostable α-Amylases, stirring mixing is added in suspension
After be warming up to 95 DEG C, insulation enzymolysis 5h, after enzymolysis at a temperature of 160 DEG C enzyme denaturing 6h, be cooled to 55 DEG C after enzyme denaturing, and with quality point
Several 15% salt acid for adjusting pH value are 5.5, sequentially add 0.5g enzymatic activitys 200u/g beta amylase and 0.3g enzymatic activitys 20u/ after regulation
G pullulanase, stirring mixing 3h, after stirring, enzyme denaturing 15min, filtration after enzyme denaturing at a temperature of 200 DEG C, collects filtrate, measures
5% formalin of 100mL mass fractions is added in there-necked flask, is adjusted pH value with 15% sodium hydroxide solution of mass fraction and is
10.0, there-necked flask is put in oil bath pan, 80 DEG C are heated to, and 0.7g Boraxs is added after insulated and stirred mixing 10min, to Borax
50g tripolycyanamide and the above-mentioned filtrates of 80g are added after dissolving, with 3 DEG C/min ramps to 100 DEG C, insulated and stirred 3h uses quality
It is 10.0 that 5% sodium hydroxide solution of fraction adjusts pH value, is cooled to room temperature, obtains dope after regulation；It is above-mentioned viscous that 80g is weighed respectively
Thick thing, 0.2g platinum dioxides, 0.10g vinyl-terminated silicone fluids, under 1000r/min rotating speeds, stirring mixing 30min, obtains component A；Most
80g vinyl-terminated silicone fluid, 8g containing hydrogen silicone oil are weighed afterwards respectively, and under 1000r/min rotating speeds, stirring mixing 30min, obtains component B,
Component A and component B in mass ratio 1 by above-mentioned preparation:1 mixing, with vacuum defoamation after 800r/min rotating speed mixing 30min
5min, you can obtain high viscosity aging resistance casting glue.
High viscosity aging resistance casting glue prepared by the present invention is injected in LED shaping mold cavities first, be inserted into pressure welding good
LED support be inserted into after the completion of, be put in baking oven and solidified, it is 120 DEG C to control temperature in baking oven, after solidification 45min,
LED is deviate from from die cavity.After testing, the high viscosity aging resistance embedding adhesiveness that prepared by the present invention reaches 5000mPa
S, heat conductivity reach 1.7W/m k, and hardness reaches 65H, and tensile strength reaches 3.7MPa.
Example 2
Weigh 200g Fructus Hordei Germinatus first, be placed in beater after peeling, and add 100g deionized waters, with 3 layers of yarn after beating 30min
Cloth is filtered, and collects filtering residue, filtering residue is put in baking oven, 6h is dried at 60 DEG C, and dried filtering residue is added super micron mill
Middle crushing, crosses 150 mesh sieves, obtains powder；By above-mentioned powder in mass ratio 1:5 are mixed with pH6.5 NaAc_HAc buffer solutions,
Suspension is obtained after stirring mixing 20min, and 0.3g enzymatic activity 100u/g Thermostable α-Amylases, stirring mixing is added in suspension
After be warming up to 90 DEG C, insulation enzymolysis 3h, after enzymolysis at a temperature of 140 DEG C enzyme denaturing 4h, be cooled to 50 DEG C after enzyme denaturing, and with quality point
Several 15% salt acid for adjusting pH value are 5.0, sequentially add 0.3g enzymatic activitys 100u/g beta amylase and 0.1g enzymatic activitys 10u/ after regulation
G pullulanase, stirring mixing 2h, after stirring, enzyme denaturing 10min, filtration after enzyme denaturing at a temperature of 210 DEG C, collects filtrate, measures
5% formalin of 80mL mass fractions is added in there-necked flask, and it is 9.0 to adjust pH value with 15% sodium hydroxide solution of mass fraction,
There-necked flask is put in oil bath pan, 70 DEG C are heated to, and 0.5g Boraxs is added after insulated and stirred mixing 5min, to Borax dissolving
30g tripolycyanamide and the above-mentioned filtrates of 60g is added, with 2 DEG C/min ramps to 90 DEG C, insulated and stirred 2h, with mass fraction 5%
It is 9.0 that sodium hydroxide solution adjusts pH value, is cooled to room temperature, obtains dope after regulation；Weigh respectively the above-mentioned dopes of 60g,
0.1g platinum dioxides, 0.08g vinyl-terminated silicone fluids, under 800r/min rotating speeds, stirring mixing 25min, obtains component A；Finally distinguish
60g vinyl-terminated silicone fluids, 6g containing hydrogen silicone oils is weighed, stirring mixing 25min, obtains component B, by above-mentioned system under 800r/min rotating speeds
Standby component A and component B in mass ratio 1:1 mixing, with vacuum defoamation 3min after 600r/min rotating speed mixing 20min, you can
Arrive high viscosity aging resistance casting glue.
High viscosity aging resistance casting glue prepared by the present invention is injected in LED shaping mold cavities first, be inserted into pressure welding good
LED support be inserted into after the completion of, be put in baking oven and solidified, it is 128 DEG C to control temperature in baking oven, after solidification 47min,
LED is deviate from from die cavity.After testing, the high viscosity aging resistance embedding adhesiveness that prepared by the present invention reaches 7000mPa
S, heat conductivity reach 2.0W/m k, and hardness reaches 68H, and tensile strength reaches 4.0MPa.
Example 3
Weigh 250g Fructus Hordei Germinatus first, be placed in beater after peeling, and add 150g deionized waters, with 3 layers of yarn after beating 35min
Cloth is filtered, and collects filtering residue, filtering residue is put in baking oven, 7h is dried at 65 DEG C, and dried filtering residue is added super micron mill
Middle crushing, crosses 160 mesh sieves, obtains powder；By above-mentioned powder in mass ratio 1:5 are mixed with pH6.5 NaAc_HAc buffer solutions,
Suspension is obtained after stirring mixing 25min, and 0.4g enzymatic activity 150u/g Thermostable α-Amylases, stirring mixing is added in suspension
After be warming up to 92 DEG C, insulation enzymolysis 4h, after enzymolysis at a temperature of 150 DEG C enzyme denaturing 5h, be cooled to 52 DEG C after enzyme denaturing, and with quality point
Several 15% salt acid for adjusting pH value are 5.2, sequentially add 0.4g enzymatic activitys 150u/g beta amylase and 0.2g enzymatic activitys 15u/ after regulation
G pullulanase, stirring mixing 2h, after stirring, enzyme denaturing 12min, filtration after enzyme denaturing at a temperature of 220 DEG C, collects filtrate, measures
5% formalin of 90mL mass fractions is added in there-necked flask, and it is 9.5 to adjust pH value with 15% sodium hydroxide solution of mass fraction,
There-necked flask is put in oil bath pan, 75 DEG C are heated to, and 0.6g Boraxs is added after insulated and stirred mixing 7min, to Borax dissolving
35g tripolycyanamide and the above-mentioned filtrates of 70g is added, with 2 DEG C/min ramps to 95 DEG C, insulated and stirred 2h, with mass fraction 5%
It is 9.5 that sodium hydroxide solution adjusts pH value, is cooled to room temperature, obtains dope after regulation；Weigh respectively the above-mentioned dopes of 70g,
0.1g platinum dioxides, 0.09g vinyl-terminated silicone fluids, under 900r/min rotating speeds, stirring mixing 27min, obtains component A；Finally distinguish
70g vinyl-terminated silicone fluids, 7g containing hydrogen silicone oils is weighed, stirring mixing 27min, obtains component B, by above-mentioned system under 900r/min rotating speeds
Standby component A and component B in mass ratio 1:1 mixing, with vacuum defoamation 4min after 700r/min rotating speed mixing 25min, you can
Arrive high viscosity aging resistance casting glue.
High viscosity aging resistance casting glue prepared by the present invention is injected in LED shaping mold cavities first, be inserted into pressure welding good
LED support be inserted into after the completion of, be put in baking oven and solidified, it is 135 DEG C to control temperature in baking oven, after solidification 60min,
LED is deviate from from die cavity.After testing, the high viscosity aging resistance embedding adhesiveness that prepared by the present invention reaches 8500mPa
S, heat conductivity reach 2.5W/m k, and hardness reaches 70H, and tensile strength reaches 4.5MPa.
Claims (1)
1. a kind of preparation method of high viscosity aging resistance casting glue, it is characterised in that concrete preparation process is：
（1）Weigh 200～300g Fructus Hordei Germinatus, be placed in beater after peeling, and add 100～200g deionized waters, beating 30～
With 3 layers of filtered through gauze after 40min, filtering residue is collected, filtering residue is put in baking oven, at 60～70 DEG C, dry 6～8h, after drying
Filtering residue add super micron mill in crush, cross 150～170 mesh sieves, obtain powder；
（2）By above-mentioned powder in mass ratio 1:5 are mixed with pH6.5 NaAc_HAc buffer solutions, stirring 20～30min of mixing
Obtain suspension afterwards, 0.3～0.5g enzymatic activity 100～200u/g Thermostable α-Amylases are added in suspension, after stirring mixing
Be warming up to 90～95 DEG C, insulation enzymolysis 3～5h, after enzymolysis at a temperature of 140～160 DEG C 4～6h of enzyme denaturing, be cooled to 50 after enzyme denaturing
～55 DEG C, and be 5.0～5.5 with 15% salt acid for adjusting pH value of mass fraction, 0.3～0.5g enzymatic activitys 100 are sequentially added after regulation
～200u/g beta amylases and 0.1～0.3g enzymatic activity 10～20u/g pullulanase, stirring 2～3h of mixing, 200 after stirring
10～15min of enzyme denaturing at a temperature of～220 DEG C, filters after enzyme denaturing, collects filtrate,
（3）Measure 80～100mL mass fractions, 5% formalin to add in there-necked flask, molten with 15% sodium hydroxide of mass fraction
Liquid adjust pH value be 9.0～10.0, there-necked flask is put in oil bath pan, 70～80 DEG C are heated to, insulated and stirred mixing 5～
0.5～0.7g Boraxs are added after 10min, add 30～50g tripolycyanamide and the above-mentioned filtrates of 60～80g, with 2 to Borax dissolving
～3 DEG C/min ramps to 90～100 DEG C, 2～3h of insulated and stirred, adjusting pH value with 5% sodium hydroxide solution of mass fraction is
9.0～10.0, room temperature is cooled to after regulation, obtain dope；
（4）60～80g above-mentioned dope, 0.1～0.2g platinum dioxide, 0.08～0.10g vinyl-terminated silicone fluid are weighed respectively,
Under 800～1000r/min rotating speeds, 25～30min of stirring mixing, obtains component A；
（5）Weigh 60～80g vinyl-terminated silicone fluids, 6～8g containing hydrogen silicone oils respectively, stir under 800～1000r/min rotating speeds mixed
25～30min is closed, component B is obtained, by component A and component B in mass ratio 1 of above-mentioned preparation:1 mixing, is turned with 600～800r/min
3～5min of vacuum defoamation after speed 20～30min of mixing, you can obtain high viscosity aging resistance casting glue.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107974039A (en) * | 2017-12-14 | 2018-05-01 | 滁州德铭塑胶有限公司 | A kind of smooth melamine resin plastic tableware preparation method in surface |
| CN108192279A (en) * | 2017-12-14 | 2018-06-22 | 滁州德铭塑胶有限公司 | A kind of preparation method of high temperature resistant melamine resin plastic tableware |
| CN108587539A (en) * | 2018-04-23 | 2018-09-28 | 广西大学 | The preparation method of glucose modified melamine formaldehyde resin wood adhesive |
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| CN101851651A (en) * | 2010-03-25 | 2010-10-06 | 江南大学 | Biosynthesis method for temperature-resistant dendritic slow-digestion starch |
| CN102850804A (en) * | 2012-08-22 | 2013-01-02 | 深圳天鼎精细化工制造有限公司 | Transparent two-component organic silicon pouring sealant for LED and preparation method thereof |
| CN103666350A (en) * | 2013-12-11 | 2014-03-26 | 广西大学 | Maltose-melamine-formaldehyde copolycondensation resin wood adhesive and preparation method thereof |
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| CN101851651A (en) * | 2010-03-25 | 2010-10-06 | 江南大学 | Biosynthesis method for temperature-resistant dendritic slow-digestion starch |
| CN102850804A (en) * | 2012-08-22 | 2013-01-02 | 深圳天鼎精细化工制造有限公司 | Transparent two-component organic silicon pouring sealant for LED and preparation method thereof |
| CN103666350A (en) * | 2013-12-11 | 2014-03-26 | 广西大学 | Maltose-melamine-formaldehyde copolycondensation resin wood adhesive and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107974039A (en) * | 2017-12-14 | 2018-05-01 | 滁州德铭塑胶有限公司 | A kind of smooth melamine resin plastic tableware preparation method in surface |
| CN108192279A (en) * | 2017-12-14 | 2018-06-22 | 滁州德铭塑胶有限公司 | A kind of preparation method of high temperature resistant melamine resin plastic tableware |
| CN108587539A (en) * | 2018-04-23 | 2018-09-28 | 广西大学 | The preparation method of glucose modified melamine formaldehyde resin wood adhesive |
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Application publication date: 20170315 |