CN106317279B - A kind of preparation method of weather-proof toughness white glue with vinyl - Google Patents
A kind of preparation method of weather-proof toughness white glue with vinyl Download PDFInfo
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- CN106317279B CN106317279B CN201610721509.4A CN201610721509A CN106317279B CN 106317279 B CN106317279 B CN 106317279B CN 201610721509 A CN201610721509 A CN 201610721509A CN 106317279 B CN106317279 B CN 106317279B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F118/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid
- C08F118/02—Esters of monocarboxylic acids
- C08F118/04—Vinyl esters
- C08F118/08—Vinyl acetate
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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
- C09J131/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid, or of a haloformic acid; Adhesives based on derivatives of such polymers
- C09J131/02—Homopolymers or copolymers of esters of monocarboxylic acids
- C09J131/04—Homopolymers or copolymers of vinyl acetate
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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
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Abstract
The invention discloses a kind of preparation methods of weather-proof toughness white glue with vinyl, belong to white glue with vinyl preparation technical field.The present invention take Fresh Laminaria Japonica shred plus boiling boiling, it grinds and kelp slurries is made, with the mixed fermentations such as secondary settling tank activated sludge, concentration mucus is made through boiling, ultrasonic extraction, filtering and concentrating in gained mixed fermentation object, be added after glacial acetic acid etc. is stirred to react, and cold water mix, filter filtration cakes torrefaction obtains buff white solid, polyvinyl alcohol is added, then is stirred to react with vinyl acetate etc. and weather-proof toughness white glue with vinyl is made.Preparation step of the present invention is simple, at low cost, and products obtained therefrom durability is good, and curing time is short；Thallus Laminariae (Thallus Eckloniae) extract part substitution polyvinyl alcohol preparation white glue with vinyl is made full use of, it is with strong points, effectively increase white glue with vinyl weatherability and impact resistance.
Description
Technical field
The present invention relates to a kind of preparation methods of weather-proof toughness white glue with vinyl, belong to white glue with vinyl preparation technical field.
Background technique
White glue with vinyl is one of most wide purposes, dosage maximum, water soluble adhesive with the longest history, is by vinyl acetate list
A kind of body thermoplastic adhesives prepared by aggregated reaction under initiator effect.It is normal temperature solidified, solidification is very fast, bonding is strong
It spends higher.It can be widely applied to bonding paper products (wallpaper), the adhesive of water-repellent paint and timber can also be made, can also widely be used
In printing bookbinding and Furniture manufacture, the binder as paper, timber, cloth, leather, ceramics etc. can also make phenolic resin, ureaformaldehyde
The modifying agent of the binders such as resin, for manufacturing Polyvinyl acetate latex paint etc..White glue with vinyl is to use polyvinyl alcohol to protect at present
Colloid is protected, is obtained by vinyl acetate by radical reaction polymerization.But gained white glue with vinyl can generate creep at high temperature,
(- 5 DEG C or less) frost resistance is poor when low temperature, and impact resistance (toughness) is poor.The main reason for creep, is in white glue with vinyl mainly
The group for playing gluing is the strand containing great amount of hydroxy group, hydroxyl inherently hydrophilic radical, in the case where meeting water, hydroxyl
Basic body and macromolecular chain migrate together, cause the intensity of glue-line to decline, so that creep.This defect is difficult to meet practical application
Requirement, also greatly limit the application of white glue with vinyl.To meet the needs of society is growing to white glue with vinyl, reduce
Product cost improves quality, it would therefore be highly desirable to research and develop the Virgin's milk of a kind of water resistance, frost resistance and good weatherability, low cost
Glue.
Summary of the invention
The technical problems to be solved by the invention: creep can be generated at high temperature for white glue with vinyl, in low temperature (- 5
DEG C or less) frost resistance is poor, and the drawback that impact resistance (toughness) is poor, at high cost, provide one kind take Fresh Laminaria Japonica shred plus
Boiling boiling, grinds and kelp slurries is made, and with the mixed fermentations such as secondary settling tank activated sludge, gained mixed fermentation object is through boiling, ultrasound
It extracts, the obtained concentration mucus of filtering and concentrating, after addition acetic anhydride and glacial acetic acid etc. are stirred to react, with cold water mix, filters to obtain filter
Biscuit it is dry buff white solid, polyvinyl alcohol is added, then be stirred to react with vinyl acetate etc. and weather-proof toughness Virgin's milk is made
The method of glue.Preparation step of the present invention is simple, at low cost；Thallus Laminariae (Thallus Eckloniae) extract part substitution polyvinyl alcohol is made full use of to prepare Virgin's milk
Glue, with strong points, creep can be generated at high temperature by efficiently solving it, and in low temperature, frost resistance is poor, and poor toughness
Problem.
In order to solve the above technical problems, the present invention is using technical solution as described below:
(1) 300~500g of Fresh Laminaria Japonica is weighed, is manually shredded into 3 × 3cm fragment, then the addition of gained fragment is filled 2
In the cast iron pan of~3L deionized water, 10~15min is boiled in heating, filters while hot, is then transferred to filtering gained kelp fragment
15~20min is ground in stone mill, is mixed into 1~2L deionized water during the grinding process, is collected to obtain kelp slurries；
(2) the above-mentioned gained kelp slurries of 800~1000mL are measured, the fermentor for filling 300~400mL deionized water is added
In, 80~100g secondary settling tank activated sludge is added, fermenter stirrer is opened, is stirred with 600~800r/min revolving speed
After 10~15min, compressed air is passed through into fermentor with 3~5mL/min rate, in temperature be 40~42 DEG C, revolving speed 120
Under the conditions of~160r/min, ferment 24~36h, obtains mixed fermentation object；
(3) above-mentioned gained mixed fermentation object is transferred in steamer, 15~20min of boiling under the conditions of 90~95 DEG C, then
It is transferred to sonic oscillation instrument while hot, with 200~240W power 15~20min of ultrasonic extraction, filtering removes filter residue, obtains fermentation liquid, then
It is transferred in Rotary Evaporators, under the conditions of temperature is 75~80 DEG C, the 1/3 of concentrated by rotary evaporation to original volume, obtain concentration mucus；
(4) it successively measures the above-mentioned gained of 100~120mL and mucus, 8~10mL glacial acetic acid and 6~8mL acetic anhydride is concentrated, add
Enter in three-necked flask, then three-necked flask is transferred to digital display and is tested the speed in constant temperature blender with magnetic force, adjusts the temperature to 35~40 DEG C, revolving speed
To 350~400r/min, under constant temperature stirring, dropwise addition 3~5mL mass fraction is 98% sulfuric acid, wait be added dropwise, heating
80~85 DEG C are warming up to, insulated and stirred reacts 6~8h；
(5) to the end of reacting, material in three-necked flask is poured into the burning for filling that 500~600mL temperature is 6~8 DEG C of cold water
In cup, it is stirred 3~5min with glass bar, is filtered, filtrate is removed, gained filter cake is washed with deionized 3~5 times, with
Filter cake is transferred in vacuum oven afterwards, dry 6~8h under the conditions of being 65~70 DEG C in temperature obtains buff white solid；
(6) the above-mentioned gained buff white solid of 100~120g and 100~120g polyvinyl alcohol are successively weighed, addition fills 600
In the beaker of~800mL deionized water, then place the beaker digital display and test the speed in constant temperature blender with magnetic force, in temperature be 85~90
DEG C, under the conditions of revolving speed is 400~500r/min, constant temperature stirring is completely dissolved up to solid, obtains mixed solution；
(7) according to parts by weight, 45~50 parts of vinyl acetates are successively taken, 25~30 parts of above-mentioned gained mixed solutions, 180~
200 parts of deionized waters and 0.5~0.8 part of ammonium persulfate, by taken mixed solution, reaction kettle is added in ammonium persulfate and deionized water
In, it is 75~80 DEG C in temperature, under the conditions of revolving speed is 400~600r/min, constant temperature is stirred 4~6min, stirs in constant temperature
Under state, taken vinyl acetate is added dropwise, control time for adding is 60~80min, continues constant temperature and is stirred to react 6~8h, reaction knot
Beam is stood, and cooled to room temperature obtains white emulsion, as weather-proof toughness white glue with vinyl.
Application method of the invention: weather-proof toughness white glue with vinyl produced by the present invention is used for ceramic tile and cement wall (ground) face
Stickup, white glue with vinyl mixes with tap water and mixed well by 1:3 in mass ratio, mixture is made, in mass ratio by mixture and cement
1:5 is mixed into paste glue, paste liquid glue is scraped on cement wall (ground) face, then the ceramic tile that need to be pasted is pressed on coated face i.e.
It can.The white glue with vinyl weatherability and impact resistance are good, and 24~30h is freezed under the conditions of -6~-4 DEG C, and no freezeout occurs, shearing
Intensity is up to 3.28~3.86MPa, and viscosity is 12.5~13.2Pas, and adhesive strength is 86~99MPa at 25 DEG C, is worth pushing away
Extensively with use.
The present invention is compared with other methods, and advantageous effects are:
(1) preparation step of the present invention is simple, at low cost, and products obtained therefrom durability is good, and curing time is short；
(2) Thallus Laminariae (Thallus Eckloniae) extract part substitution polyvinyl alcohol preparation white glue with vinyl is made full use of, it is with strong points, it effectively increases white
Latex weatherability and impact resistance.
Specific embodiment
300~500g of Fresh Laminaria Japonica is weighed first, is manually shredded into 3 × 3cm fragment, then the addition of gained fragment is filled
In the cast iron pan of 2~3L deionized water, 10~15min is boiled in heating, filters while hot, is then transferred to filtering gained kelp fragment
15~20min is ground in stone mill, is mixed into 1~2L deionized water during the grinding process, is collected to obtain kelp slurries；Measurement 800~
The above-mentioned gained kelp slurries of 1000mL are added in the fermentor for filling 300~400mL deionized water, add 80~100g bis-
Heavy pond activated sludge opens fermenter stirrer, after being stirred 10~15min with 600~800r/min revolving speed, with 3~
5mL/min rate is passed through compressed air into fermentor, in temperature be 40~42 DEG C, revolving speed be 120~160r/min under the conditions of,
Ferment 24~36h, obtains mixed fermentation object；Above-mentioned gained mixed fermentation object is transferred in steamer, the boiling under the conditions of 90~95 DEG C
15~20min is then transferred to sonic oscillation instrument while hot, and with 200~240W power 15~20min of ultrasonic extraction, filtering removes filter
Slag obtains fermentation liquid, then is transferred in Rotary Evaporators, under the conditions of temperature is 75~80 DEG C, concentrated by rotary evaporation to original volume
1/3, obtain concentration mucus；Then it successively measures the above-mentioned gained of 100~120mL and mucus, 8~10mL glacial acetic acid and 6~8mL vinegar is concentrated
Acid anhydrides is added in three-necked flask, then three-necked flask is transferred to digital display and is tested the speed in constant temperature blender with magnetic force, adjusts the temperature to 35~40
DEG C, revolving speed to 350~400r/min, under constant temperature stirring, dropwise addition 3~5mL mass fraction is 98% sulfuric acid, wait drip
Finish, is heated to 80~85 DEG C, insulated and stirred reacts 6~8h；To the end of reacting, material in three-necked flask is poured into and is filled
500~600mL temperature is to be stirred 3~5min with glass bar in the beaker of 6~8 DEG C of cold water, filters, filtrate is removed, by institute
It obtains filter cake to be washed with deionized 3~5 times, then filter cake is transferred in vacuum oven, under the conditions of temperature is 65~70 DEG C
Dry 6~8h, obtains buff white solid；Successively weigh the above-mentioned gained buff white solid of 100~120g and 100~120g polyethylene
Alcohol is added and fills in the beaker of 600~800mL deionized water, then places the beaker digital display and test the speed in constant temperature blender with magnetic force, in
Temperature is 85~90 DEG C, and under the conditions of revolving speed is 400~500r/min, constant temperature stirring is completely dissolved up to solid, obtains mixed solution；
Finally according to parts by weight, 45~50 parts of vinyl acetates are successively taken, 25~30 parts of above-mentioned gained mixed solutions, 180~200 parts are gone
Ionized water and 0.5~0.8 part of ammonium persulfate, by taken mixed solution, ammonium persulfate and deionized water are added in reaction kettle, Yu Wen
Degree is 75~80 DEG C, and under the conditions of revolving speed is 400~600r/min, constant temperature is stirred 4~6min, under constant temperature stirring,
Taken vinyl acetate is added dropwise, control time for adding is 60~80min, continues constant temperature and is stirred to react 6~8h, and reaction terminates, it stands,
Cooled to room temperature obtains white emulsion, as weather-proof toughness white glue with vinyl.
Example 1
Fresh Laminaria Japonica 300g is weighed first, is manually shredded into 3 × 3cm fragment, then the addition of gained fragment is filled into 2L
In the cast iron pan of ionized water, 10min is boiled in heating, filters while hot, and then filtering gained kelp fragment is transferred in stone mill and is ground
15min is mixed into 1L deionized water during the grinding process, collects to obtain kelp slurries；The above-mentioned gained kelp slurries of 800mL are measured, are added
In the fermentor for entering to fill 300mL deionized water, 80g secondary settling tank activated sludge is added, opens fermenter stirrer, with
After 600r/min revolving speed is stirred 10min, compressed air is passed through into fermentor with 3mL/min rate, in temperature be 40 DEG C,
Under the conditions of revolving speed is 120r/min, fermentation for 24 hours, obtains mixed fermentation object；Above-mentioned gained mixed fermentation object is transferred in steamer, in 90
Boiling 15min under the conditions of DEG C is then transferred to sonic oscillation instrument while hot, and with 200W power ultrasonic extraction 15min, filtering removes filter
Slag obtains fermentation liquid, then is transferred in Rotary Evaporators, under the conditions of temperature is 75 DEG C, the 1/3 of concentrated by rotary evaporation to original volume,
Mucus must be concentrated；Then it successively measures the above-mentioned gained of 100mL and mucus, 8mL glacial acetic acid and 6mL acetic anhydride is concentrated, three mouthfuls of burnings are added
In bottle, then three-necked flask is transferred to digital display and is tested the speed in constant temperature blender with magnetic force, adjusts the temperature to 35 DEG C, revolving speed to 350r/min,
Under constant temperature stirring, dropwise addition 3mL mass fraction is heated to 80 DEG C, insulated and stirred wait be added dropwise for 98% sulfuric acid
React 6h；To the end of reacting, material in three-necked flask is poured into and is filled in the beaker that 500mL temperature is 6 DEG C of cold water, glass bar is used
It is stirred 3min, is filtered, filtrate is removed, gained filter cake is washed with deionized 3 times, filter cake is then transferred to vacuum drying
In case, dry 6h under the conditions of being 65 DEG C in temperature obtains buff white solid；Successively weigh the above-mentioned gained buff white solid of 100g and
100g polyvinyl alcohol is added and fills in the beaker of 600mL deionized water, then places the beaker digital display and test the speed constant temperature blender with magnetic force
In, it is 85 DEG C in temperature, under the conditions of revolving speed is 400r/min, constant temperature stirring is completely dissolved up to solid, obtains mixed solution；Finally
According to parts by weight, 45 parts of vinyl acetates, 25 parts of above-mentioned gained mixed solutions, 180 parts of deionized waters and 0.5 part of over cure are successively taken
Sour ammonium, by taken mixed solution, ammonium persulfate and deionized water are added in reaction kettle, in temperature be 75 DEG C, revolving speed 400r/
Under the conditions of min, constant temperature is stirred 4min, under constant temperature stirring, taken vinyl acetate is added dropwise, control time for adding is
60min continues constant temperature and is stirred to react 6h, and reaction terminates, and stands, cooled to room temperature obtains white emulsion, as weather-proof tough
Property white glue with vinyl.
Weather-proof toughness white glue with vinyl produced by the present invention is used for the stickup of ceramic tile Yu cement wall (ground) face, in mass ratio 1:
3, white glue with vinyl is mixed with tap water and is mixed well, mixture is made, mixture and cement 1:5 in mass ratio are mixed into paste glue,
Paste liquid glue is scraped on cement wall (ground) face, then the ceramic tile that need to be pasted is pressed on into coated face.The white glue with vinyl weatherability
It is good with impact resistance, it is freezed under the conditions of -6 DEG C for 24 hours, no freezeout occurs, and shear strength reaches 3.28MPa, and viscosity is
12.5Pas, adhesive strength is 86MPa at 25 DEG C, is worthy to be popularized and uses.
Example 2
Fresh Laminaria Japonica 400g is weighed first, is manually shredded into 3 × 3cm fragment, then the addition of gained fragment is filled into 3L
In the cast iron pan of ionized water, 13min is boiled in heating, filters while hot, and then filtering gained kelp fragment is transferred in stone mill and is ground
18min is mixed into 2L deionized water during the grinding process, collects to obtain kelp slurries；The above-mentioned gained kelp slurries of 900mL are measured, are added
In the fermentor for entering to fill 350mL deionized water, 90g secondary settling tank activated sludge is added, opens fermenter stirrer, with
After 700r/min revolving speed is stirred 13min, compressed air is passed through into fermentor with 4mL/min rate, in temperature be 41 DEG C,
Under the conditions of revolving speed is 140r/min, ferment 30h, obtains mixed fermentation object；Above-mentioned gained mixed fermentation object is transferred in steamer, in 93
Boiling 18min under the conditions of DEG C is then transferred to sonic oscillation instrument while hot, and with 220W power ultrasonic extraction 18min, filtering removes filter
Slag obtains fermentation liquid, then is transferred in Rotary Evaporators, under the conditions of temperature is 78 DEG C, the 1/3 of concentrated by rotary evaporation to original volume,
Mucus must be concentrated；Then it successively measures the above-mentioned gained of 110mL and mucus, 9mL glacial acetic acid and 7mL acetic anhydride is concentrated, three mouthfuls of burnings are added
In bottle, then three-necked flask is transferred to digital display and is tested the speed in constant temperature blender with magnetic force, adjusts the temperature to 38 DEG C, revolving speed to 375r/min,
Under constant temperature stirring, dropwise addition 4mL mass fraction is heated to 83 DEG C, insulated and stirred wait be added dropwise for 98% sulfuric acid
React 7h；To the end of reacting, material in three-necked flask is poured into and is filled in the beaker that 550mL temperature is 7 DEG C of cold water, glass bar is used
It is stirred 4min, is filtered, filtrate is removed, gained filter cake is washed with deionized 4 times, filter cake is then transferred to vacuum drying
In case, dry 7h under the conditions of being 68 DEG C in temperature obtains buff white solid；Successively weigh the above-mentioned gained buff white solid of 110g and
110g polyvinyl alcohol is added and fills in the beaker of 700mL deionized water, then places the beaker digital display and test the speed constant temperature blender with magnetic force
In, it is 88 DEG C in temperature, under the conditions of revolving speed is 450r/min, constant temperature stirring is completely dissolved up to solid, obtains mixed solution；Finally
According to parts by weight, 48 parts of vinyl acetates, 28 parts of above-mentioned gained mixed solutions, 190 parts of deionized waters and 0.7 part of over cure are successively taken
Sour ammonium, by taken mixed solution, ammonium persulfate and deionized water are added in reaction kettle, in temperature be 78 DEG C, revolving speed 500r/
Under the conditions of min, constant temperature is stirred 5min, under constant temperature stirring, taken vinyl acetate is added dropwise, control time for adding is
70min continues constant temperature and is stirred to react 7h, and reaction terminates, and stands, cooled to room temperature obtains white emulsion, as weather-proof tough
Property white glue with vinyl.
Weather-proof toughness white glue with vinyl produced by the present invention is used for the stickup of ceramic tile Yu cement wall (ground) face, in mass ratio 1:
3, white glue with vinyl is mixed with tap water and is mixed well, mixture is made, mixture and cement 1:5 in mass ratio are mixed into paste glue,
Paste liquid glue is scraped on cement wall (ground) face, then the ceramic tile that need to be pasted is pressed on into coated face.The white glue with vinyl weatherability
It is good with impact resistance, 27h is freezed under the conditions of -5 DEG C, no freezeout occurs, and shear strength reaches 3.57MPa, and viscosity is
12.9Pas, adhesive strength is 92MPa at 25 DEG C, is worthy to be popularized and uses.
Example 3
Fresh Laminaria Japonica 500g is weighed first, is manually shredded into 3 × 3cm fragment, then the addition of gained fragment is filled into 3L
In the cast iron pan of ionized water, 15min is boiled in heating, filters while hot, and then filtering gained kelp fragment is transferred in stone mill and is ground
20min is mixed into 2L deionized water during the grinding process, collects to obtain kelp slurries；The above-mentioned gained kelp slurries of 1000mL are measured, are added
In the fermentor for entering to fill 400mL deionized water, 100g secondary settling tank activated sludge is added, opens fermenter stirrer, with
After 800r/min revolving speed is stirred 15min, compressed air is passed through into fermentor with 5mL/min rate, in temperature be 42 DEG C,
Under the conditions of revolving speed is 160r/min, ferment 36h, obtains mixed fermentation object；Above-mentioned gained mixed fermentation object is transferred in steamer, in 95
Boiling 20min under the conditions of DEG C is then transferred to sonic oscillation instrument while hot, and with 240W power ultrasonic extraction 20min, filtering removes filter
Slag obtains fermentation liquid, then is transferred in Rotary Evaporators, under the conditions of temperature is 80 DEG C, the 1/3 of concentrated by rotary evaporation to original volume,
Mucus must be concentrated；Then it successively measures the above-mentioned gained of 120mL and mucus, 10mL glacial acetic acid and 8mL acetic anhydride is concentrated, three mouthfuls of burnings are added
In bottle, then three-necked flask is transferred to digital display and is tested the speed in constant temperature blender with magnetic force, adjusts the temperature to 40 DEG C, revolving speed to 400r/min,
Under constant temperature stirring, dropwise addition 5mL mass fraction is heated to 85 DEG C, insulated and stirred wait be added dropwise for 98% sulfuric acid
React 8h；To the end of reacting, material in three-necked flask is poured into and is filled in the beaker that 600mL temperature is 8 DEG C of cold water, glass bar is used
It is stirred 5min, is filtered, filtrate is removed, gained filter cake is washed with deionized 5 times, filter cake is then transferred to vacuum drying
In case, dry 8h under the conditions of being 70 DEG C in temperature obtains buff white solid；Successively weigh the above-mentioned gained buff white solid of 120g and
120g polyvinyl alcohol is added and fills in the beaker of 800mL deionized water, then places the beaker digital display and test the speed constant temperature blender with magnetic force
In, it is 90 DEG C in temperature, under the conditions of revolving speed is 500r/min, constant temperature stirring is completely dissolved up to solid, obtains mixed solution；Finally
According to parts by weight, 50 parts of vinyl acetates, 30 parts of above-mentioned gained mixed solutions, 200 parts of deionized waters and 0.8 part of over cure are successively taken
Sour ammonium, by taken mixed solution, ammonium persulfate and deionized water are added in reaction kettle, in temperature be 80 DEG C, revolving speed 600r/
Under the conditions of min, constant temperature is stirred 6min, under constant temperature stirring, taken vinyl acetate is added dropwise, control time for adding is
80min continues constant temperature and is stirred to react 8h, and reaction terminates, and stands, cooled to room temperature obtains white emulsion, as weather-proof tough
Property white glue with vinyl.
Weather-proof toughness white glue with vinyl produced by the present invention is used for the stickup of ceramic tile Yu cement wall (ground) face, in mass ratio 1:
3, white glue with vinyl is mixed with tap water and is mixed well, mixture is made, mixture and cement 1:5 in mass ratio are mixed into paste glue,
Paste liquid glue is scraped on cement wall (ground) face, then the ceramic tile that need to be pasted is pressed on into coated face.The white glue with vinyl weatherability
It is good with impact resistance, 30h is freezed under the conditions of -4 DEG C, no freezeout occurs, and shear strength reaches 3.86MPa, and viscosity is
13.2Pas, adhesive strength is 99MPa at 25 DEG C, is worthy to be popularized and uses.
Claims (1)
1. a kind of preparation method of weather-proof toughness white glue with vinyl, it is characterised in that specific preparation step are as follows:
(1) 300~500g of Fresh Laminaria Japonica is weighed, is manually shredded into 3 × 3cm fragment, then the addition of gained fragment is filled into 2~3L
In the cast iron pan of deionized water, 10~15min is boiled in heating, filters while hot, and filtering gained kelp fragment is then transferred to stone mill
15~20min of middle grinding, is mixed into 1~2L deionized water during the grinding process, collects to obtain kelp slurries；
(2) the above-mentioned gained kelp slurries of 800~1000mL are measured, are added in the fermentor for filling 300~400mL deionized water,
It adds 80~100g secondary settling tank activated sludge, opens fermenter stirrer, 10 are stirred with 600~800r/min revolving speed~
After 15min, compressed air is passed through into fermentor with 3~5mL/min rate, in temperature be 40~42 DEG C, revolving speed be 120~
Under the conditions of 160r/min, ferment 24~36h, obtains mixed fermentation object；
(3) above-mentioned gained mixed fermentation object is transferred in steamer, 15~20min of boiling under the conditions of 90~95 DEG C, then while hot
Be transferred to sonic oscillation instrument, with 200~240W power 15~20min of ultrasonic extraction, filtering removes filter residue, obtain fermentation liquid, then by its
It is transferred in Rotary Evaporators, under the conditions of temperature is 75~80 DEG C, the 1/3 of concentrated by rotary evaporation to original volume, obtain concentration mucus；
(4) it successively measures the above-mentioned gained of 100~120mL and mucus, 8~10mL glacial acetic acid and 6~8mL acetic anhydride is concentrated, be added three
In mouthful flask, then three-necked flask is transferred to digital display and is tested the speed in constant temperature blender with magnetic force, adjusts the temperature to 35~40 DEG C, revolving speed is extremely
350~400r/min, under constant temperature stirring, dropwise addition 3~5mL mass fraction is 98% sulfuric acid, and wait be added dropwise, heating is risen
For temperature to 80~85 DEG C, insulated and stirred reacts 6~8h；
(5) to the end of reacting, material in three-necked flask is poured into and is filled in the beaker that 500~600mL temperature is 6~8 DEG C of cold water,
It is stirred 3~5min with glass bar, is filtered, filtrate is removed, gained filter cake is washed with deionized 3~5 times, it then will filter
Cake is transferred in vacuum oven, and dry 6~8h under the conditions of being 65~70 DEG C in temperature obtains buff white solid；
(6) the above-mentioned gained buff white solid of 100~120g and 100~120g polyvinyl alcohol are successively weighed, addition fills 600~
In the beaker of 800mL deionized water, then place the beaker digital display and test the speed in constant temperature blender with magnetic force, in temperature be 85~90 DEG C,
Under the conditions of revolving speed is 400~500r/min, constant temperature stirring is completely dissolved up to solid, obtains mixed solution；
(7) according to parts by weight, 45~50 parts of vinyl acetates are successively taken, 25~30 parts of above-mentioned gained mixed solutions, 180~200
Part deionized water and 0.5~0.8 part of ammonium persulfate, by taken mixed solution, ammonium persulfate and deionized water are added in reaction kettle,
It is 75~80 DEG C in temperature, under the conditions of revolving speed is 400~600r/min, constant temperature is stirred 4~6min, in constant temperature stirring
Under, taken vinyl acetate is added dropwise, control time for adding is 60~80min, continues constant temperature and is stirred to react 6~8h, reaction terminates, quiet
It sets, cooled to room temperature, obtains white emulsion, as weather-proof toughness white glue with vinyl.
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