CN106317279A - Method for preparing weather-proof tough white emulsion - Google Patents
Method for preparing weather-proof tough white emulsion Download PDFInfo
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- CN106317279A CN106317279A CN201610721509.4A CN201610721509A CN106317279A CN 106317279 A CN106317279 A CN 106317279A CN 201610721509 A CN201610721509 A CN 201610721509A CN 106317279 A CN106317279 A CN 106317279A
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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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- Chemical Kinetics & Catalysis (AREA)
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a method for preparing weather-proof tough white emulsion, and belongs to the technical field of white emulsion preparation. Fresh kelp is cut into pieces, water is added to be boiled, grinding is carried out, kelp pulp is prepared, the kelp pulp, secondary sedimentation tank activated sludge and the like are mixed and fermented, and the obtained mixed fermented product is prepared into concentrated slime through boiling, ultrasonic extraction and filtering concentration; glacial acetic acid and the like are added, after stirring for reacting, the product is mixed with cold water, filtering is carried out to obtain a filter cake, the filter cake is dried to obtain maize-yellow solids, polyvinyl alcohol is added for mixing, the mixture, vinyl acetate and the like are stirred for reacting, and the weather-proof tough white emulsion is prepared. The preparation steps are simple, cost is low, and the obtained product is good in durability and short in curing time. Kelp extract is fully utilized for partially replacing polyvinyl alcohol to prepare the white emulsion, pertinency is high, and the weather fastness and impact resistance of the white emulsion are effectively improved.
Description
Technical field
The present invention relates to the preparation method of a kind of weather resistant toughness white glue with vinyl, belong to white glue with vinyl preparing technical field.
Background technology
White glue with vinyl is one of water soluble adhesive that purposes is the widest, consumption is maximum, with the longest history, is by vinyl acetate list
Body aggregated reaction and prepared a kind of thermoplastic adhesives under initiator effect.Normal temperature solidified, solidify very fast, bonding by force
Spend higher.Can be widely applied to bonding paper products (wallpaper), it is possible to make the adhesive of water-repellent paint and timber, it is possible to use widely
In printing bookbinding and Furniture manufacture, as the adhesive of paper, timber, cloth, leather, pottery etc., phenolic resin, urea aldehyde also can be made
The modifying agent of the adhesive such as resin, is used for manufacturing Polyvinyl acetate latex paint etc..White glue with vinyl is to use polyvinyl alcohol for protecting at present
Protect colloid, vinyl acetate be polymerized by radical reaction and obtain.But gained white glue with vinyl at high temperature can produce creep,
During low temperature, (less than-5 DEG C) frost resistance is poor, and resistance to impact (toughness) is poor.Main reason is that in white glue with vinyl of creep is main
The group playing gluing effect is the strand containing great amount of hydroxy group, hydroxyl inherently hydrophilic group, in the case of meeting water, and hydroxyl
Basic body migrates together with macromolecular chain, causes the intensity of glue-line to decline, so that creep.This defect is difficult to meet reality application
Requirement, also greatly limit the application of white glue with vinyl.For the demand that satisfied society is growing to white glue with vinyl, reduce
Product cost, raising quality, it would therefore be highly desirable to research and develop the Virgin's milk of a kind of resistance to water, frost resistance and good weatherability, low cost
Glue.
Summary of the invention
The technical problem to be solved: at high temperature can produce creep for white glue with vinyl, when low temperature (-5
Below DEG C) frost resistance is poor, and resistance to impact (toughness) is poor, the drawback that cost is high, it is provided that and one takes Fresh Laminaria Japonica and shreds and add
Water boil, grinds and prepares Thallus Laminariae (Thallus Eckloniae) serosity, and the mixed fermentation such as second pond activated sludge, and gained mixed fermentation thing is through steaming and decocting, ultrasonic
Extract, filtering and concentrating prepares and concentrates mucus, after adding the stirring reaction such as acetic anhydride and glacial acetic acid, with cold water mix, filters to obtain filter
Cookies is dry obtains buff white solid, adds polyvinyl alcohol, then stirs the prepared weather resistant toughness Virgin's milk of reaction with vinyl acetate etc.
The method of glue.Preparation process of the present invention is simple, low cost；Make full use of Thallus Laminariae (Thallus Eckloniae) extract part replacement polyvinyl alcohol and prepare Virgin's milk
Glue, with strong points, efficiently solve it and at high temperature can produce creep, when low temperature, frost resistance is poor, and poor toughness
Problem.
For solving above-mentioned technical problem, the present invention uses the technical scheme as described below to be:
(1) weigh Fresh Laminaria Japonica 300～500g, through manually shredding into 3 × 3cm fragment, then the addition of gained fragment is filled 2～3L
In the cast iron pan of deionized water, heated and boiled 10～15min, filtered while hot, subsequently filtration gained Thallus Laminariae (Thallus Eckloniae) fragment is proceeded to stone grinder
Middle grinding 15～20min, is mixed into 1～2L deionized water in process of lapping, collects to obtain Thallus Laminariae (Thallus Eckloniae) serosity；
(2) measure 800～1000mL above-mentioned gained Thallus Laminariae (Thallus Eckloniae) serosity, add in the fermentation tank filling 300～400mL deionized waters,
Add 80～100g second pond activated sludge, open fermenter stirrer, with 600～800r/min rotating speeds stirring mixing 10～
After 15min, in fermentation tank, be passed through compressed air with 3～5mL/min speed, be 40～42 DEG C in temperature, rotating speed be 120～
Under the conditions of 160r/min, fermentation 24～36h, obtain mixed fermentation thing；
(3) above-mentioned gained mixed fermentation thing is proceeded in steamer, steaming and decocting 15～20min under the conditions of 90～95 DEG C, the most while hot
Proceed to sonic oscillation instrument, extract 15～20min with 200～240W power ultrasonics, filter, remove filtering residue, obtain fermentation liquid, then by it
Proceed 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) measure 100～120mL above-mentioned gained successively and concentrate mucus, 8～10mL glacial acetic acid and 6～8mL acetic anhydride, add three
In mouthful flask, then there-necked flask proceeds to digital display testing the speed in constant temperature blender with magnetic force, adjust the temperature to 35～40 DEG C, rotating speed is extremely
350～400r/min, under constant temperature stirring, dropping 3～5mL mass fractions are 98% sulphuric acid, wait to drip complete, and heating rises
Temperature is to 80～85 DEG C, and insulated and stirred reacts 6～8h；
(5) question response terminates, and is poured into by material in there-necked flask and fills in the beaker that 500～600mL temperature are 6～8 DEG C of cold water,
With Glass rod stirring mixing 3～5min, filter, remove filtrate, gained filter cake is washed with deionized 3～5 times, subsequently will filter
Cake proceeds in vacuum drying oven, is dried 6～8h, obtains buff white solid under the conditions of temperature is 65～70 DEG C；
(6) weigh 100～120g above-mentioned gained buff white solid and 100～120g polyvinyl alcohol successively, add fill 600～
In the beaker of 800mL deionized water, then beaker proceeded to digital display test the speed in constant temperature blender with magnetic force, be 85～90 DEG C in temperature,
Under the conditions of rotating speed is 400～500r/min, constant temperature stirs until solid is completely dissolved, and obtains mixed solution；
(7) count by weight, take 45～50 parts of vinyl acetates, 25～30 parts of above-mentioned gained mixed solutions, 180～200 successively
Part deionized water and 0.5～0.8 part of Ammonium persulfate., add taken mixed solution, Ammonium persulfate. and deionized water in reactor,
Being 75～80 DEG C in temperature, under the conditions of rotating speed is 400～600r/min, constant temperature stirring mixing 4～6min, at constant temperature stirring
Under, drip taken vinyl acetate, controlling time for adding is 60～80min, continues constant temperature stirring reaction 6～8h, and reaction terminates, quiet
Put, naturally cool to room temperature, obtain white emulsion, be weather resistant toughness white glue with vinyl.
The application process of the present invention: the weather resistant toughness white glue with vinyl that the present invention is prepared be used for ceramic tile and cement wall () face
Stickup, 1:3 in mass ratio, white glue with vinyl is mixed with tap water and mixes well, prepare mixture, by mixture and cement in mass ratio
1:5 is mixed into pasty state glue, pasty state sol is scraped in cement wall () on face, then the ceramic tile that need to paste is pressed on coated face i.e.
Can.This white glue with vinyl weatherability and resistance to impact are good, freezing 24～30h under the conditions of-6～-4 DEG C, occur without freezeout, shear
Intensity reaches 3.28～3.86MPa, and viscosity is 12.5～13.2Pa s, and at 25 DEG C, adhesive strength is 86～99MPa, is worth pushing away
Extensively with use.
The present invention is compared with additive method, and Advantageous Effects is:
(1) preparation process of the present invention is simple, and low cost, products obtained therefrom good endurance, hardening time is short；
(2) make full use of Thallus Laminariae (Thallus Eckloniae) extract part replacement polyvinyl alcohol and prepare white glue with vinyl, with strong points, it is effectively increased white glue with vinyl
Weatherability and resistance to impact.
Detailed description of the invention
First weigh Fresh Laminaria Japonica 300～500g, through manually shredding into 3 × 3cm fragment, then the addition of gained fragment is filled
In the cast iron pan of 2～3L deionized waters, heated and boiled 10～15min, filtered while hot, subsequently filtration gained Thallus Laminariae (Thallus Eckloniae) fragment is proceeded to
Stone grinder grinds 15～20min, process of lapping is mixed into 1～2L deionized water, collects to obtain Thallus Laminariae (Thallus Eckloniae) serosity；Measure 800～
1000mL above-mentioned gained Thallus Laminariae (Thallus Eckloniae) serosity, adds in the fermentation tank filling 300～400mL deionized waters, adds 80～100g bis-
Heavy pond activated sludge, opens fermenter stirrer, after 600～800r/min rotating speeds stirring mixing 10～15min, with 3～
5mL/min speed is passed through compressed air in fermentation tank, is 40～42 DEG C in temperature, under the conditions of rotating speed is 120～160r/min,
Fermentation 24～36h, obtains mixed fermentation thing；Above-mentioned gained mixed fermentation thing is proceeded in steamer, steaming and decocting under the conditions of 90～95 DEG C
15～20min, proceed to sonic oscillation instrument the most while hot, extract 15～20min with 200～240W power ultrasonics, filter, remove filter
Slag, obtains fermentation liquid, then is proceeded in Rotary Evaporators, and under the conditions of temperature is 75～80 DEG C, concentrated by rotary evaporation is to original volume
1/3, obtain concentration mucus；Measure 100～120mL above-mentioned gained the most successively and concentrate mucus, 8～10mL glacial acetic acid and 6～8mL vinegar
Anhydride, adds in there-necked flask, then there-necked flask proceeds to digital display tests the speed in constant temperature blender with magnetic force, adjusts the temperature to 35～40
DEG C, rotating speed to 350～400r/min, under constant temperature stirring, dropping 3～5mL mass fractions are 98% sulphuric acid, wait to drip
Finish, be heated to 80～85 DEG C, insulated and stirred reaction 6～8h；Question response terminates, and is poured into by material in there-necked flask and fills
500～600mL temperature are in the beaker of 6～8 DEG C of cold water, with Glass rod stirring mixing 3～5min, filter, remove filtrate, by institute
Obtain filter cake to be washed with deionized 3～5 times, subsequently filter cake is proceeded in vacuum drying oven, under the conditions of temperature is 65～70 DEG C
It is dried 6～8h, obtains buff white solid；Weigh 100～120g above-mentioned gained buff white solid and 100～120g polyethylene successively
Alcohol, adds and fills in the beaker of 600～800mL deionized waters, then beaker proceeds to digital display tests the speed in constant temperature blender with magnetic force, in
Temperature is 85～90 DEG C, and under the conditions of rotating speed is 400～500r/min, constant temperature stirs until solid is completely dissolved, and obtains mixed solution；
Finally counting by weight, take 45～50 parts of vinyl acetates successively, 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., add taken mixed solution, Ammonium persulfate. and deionized water in reactor, Yu Wen
Degree is 75～80 DEG C, under the conditions of rotating speed is 400～600r/min, and constant temperature stirring mixing 4～6min, under constant temperature stirring,
Dripping taken vinyl acetate, controlling time for adding is 60～80min, continues constant temperature stirring reaction 6～8h, and reaction terminates, and stands,
Naturally cool to room temperature, obtain white emulsion, be weather resistant toughness white glue with vinyl.
Example 1
First weigh Fresh Laminaria Japonica 300g, through manually shredding into 3 × 3cm fragment, then the addition of gained fragment is filled 2L deionization
In the cast iron pan of water, heated and boiled 10min, filtered while hot, proceed to filtration gained Thallus Laminariae (Thallus Eckloniae) fragment subsequently stone grinder grinds
15min, is mixed into 1L deionized water in process of lapping, collects to obtain Thallus Laminariae (Thallus Eckloniae) serosity；Measure 800mL above-mentioned gained Thallus Laminariae (Thallus Eckloniae) serosity, add
Enter to fill in the fermentation tank of 300mL deionized water, add 80g second pond activated sludge, open fermenter stirrer, with
After 600r/min rotating speed stirring mixing 10min, in fermentation tank, it is passed through compressed air with 3mL/min speed, is 40 DEG C in temperature,
Under the conditions of rotating speed is 120r/min, ferment 24h, obtains mixed fermentation thing；Above-mentioned gained mixed fermentation thing is proceeded in steamer, in 90
Steaming and decocting 15min under the conditions of DEG C, proceeds to sonic oscillation instrument the most while hot, extracts 15min with 200W power ultrasonic, filters, and removes filter
Slag, obtains fermentation liquid, then is proceeded in Rotary Evaporators, under the conditions of temperature is 75 DEG C, and the 1/3 of concentrated by rotary evaporation to original volume,
Mucus must be concentrated；Measure the above-mentioned gained of 100mL the most successively and concentrate mucus, 8mL glacial acetic acid and 6mL acetic anhydride, add three mouthfuls of burnings
In Ping, then there-necked flask proceeded to digital display test the speed in constant temperature blender with magnetic force, adjust the temperature to 35 DEG C, rotating speed to 350r/min,
Under constant temperature stirring, dropping 3mL mass fraction is 98% sulphuric acid, waits to drip complete, is heated to 80 DEG C, insulated and stirred
Reaction 6h；Question response terminates, and is poured into by material in there-necked flask and fills in the beaker that 500mL temperature is 6 DEG C of cold water, uses Glass rod
Stirring mixing 3min, filters, removes filtrate, is washed with deionized by gained filter cake 3 times, filter cake proceeds to vacuum drying subsequently
In case, under the conditions of temperature is 65 DEG C, it is dried 6h, obtains buff white solid；Weigh successively 100g above-mentioned gained buff white solid and
100g polyvinyl alcohol, adds and fills in the beaker of 600mL deionized water, then beaker proceeds to digital display tests the speed constant temperature blender with magnetic force
In, it is 85 DEG C in temperature, under the conditions of rotating speed is 400r/min, constant temperature stirs until solid is completely dissolved, and obtains mixed solution；Finally
Count by weight, take 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 successively
Acid ammonium, adds taken mixed solution, Ammonium persulfate. and deionized water in reactor, is 75 DEG C in temperature, and rotating speed is 400r/
Under the conditions of min, constant temperature stirring mixing 4min, under constant temperature stirring, drip taken vinyl acetate, controlling time for adding is
60min, continues constant temperature stirring reaction 6h, and reaction terminates, and stands, naturally cools to room temperature, obtain white emulsion, be weather resistant tough
Property white glue with vinyl.
The weather resistant toughness white glue with vinyl that the present invention is prepared be used for ceramic tile and cement wall () stickup in face, in mass ratio 1:
3, white glue with vinyl is mixed with tap water and mixes well, prepare mixture, mixture is mixed into pasty state glue with cement 1:5 in mass ratio,
Pasty state sol is scraped in cement wall () on face, then the ceramic tile that need to paste is pressed on coated face.This white glue with vinyl weatherability
Good with resistance to impact, under the conditions of-6 DEG C, freezing 24h, occurs without freezeout, and shear strength reaches 3.28MPa, and viscosity is
12.5Pa s, at 25 DEG C, adhesive strength is 86MPa, is worthy to be popularized and uses.
Example 2
First weigh Fresh Laminaria Japonica 400g, through manually shredding into 3 × 3cm fragment, then the addition of gained fragment is filled 3L deionization
In the cast iron pan of water, heated and boiled 13min, filtered while hot, proceed to filtration gained Thallus Laminariae (Thallus Eckloniae) fragment subsequently stone grinder grinds
18min, is mixed into 2L deionized water in process of lapping, collects to obtain Thallus Laminariae (Thallus Eckloniae) serosity；Measure 900mL above-mentioned gained Thallus Laminariae (Thallus Eckloniae) serosity, add
Enter to fill in the fermentation tank of 350mL deionized water, add 90g second pond activated sludge, open fermenter stirrer, with
After 700r/min rotating speed stirring mixing 13min, in fermentation tank, it is passed through compressed air with 4mL/min speed, is 41 DEG C in temperature,
Under the conditions of rotating speed is 140r/min, ferment 30h, obtains mixed fermentation thing；Above-mentioned gained mixed fermentation thing is proceeded in steamer, in 93
Steaming and decocting 18min under the conditions of DEG C, proceeds to sonic oscillation instrument the most while hot, extracts 18min with 220W power ultrasonic, filters, and removes filter
Slag, obtains fermentation liquid, then is proceeded in Rotary Evaporators, under the conditions of temperature is 78 DEG C, and the 1/3 of concentrated by rotary evaporation to original volume,
Mucus must be concentrated；Measure the above-mentioned gained of 110mL the most successively and concentrate mucus, 9mL glacial acetic acid and 7mL acetic anhydride, add three mouthfuls of burnings
In Ping, then there-necked flask proceeded to digital display test the speed in constant temperature blender with magnetic force, adjust the temperature to 38 DEG C, rotating speed to 375r/min,
Under constant temperature stirring, dropping 4mL mass fraction is 98% sulphuric acid, waits to drip complete, is heated to 83 DEG C, insulated and stirred
Reaction 7h；Question response terminates, and is poured into by material in there-necked flask and fills in the beaker that 550mL temperature is 7 DEG C of cold water, uses Glass rod
Stirring mixing 4min, filters, removes filtrate, is washed with deionized by gained filter cake 4 times, filter cake proceeds to vacuum drying subsequently
In case, under the conditions of temperature is 68 DEG C, it is dried 7h, obtains buff white solid；Weigh successively 110g above-mentioned gained buff white solid and
110g polyvinyl alcohol, adds and fills in the beaker of 700mL deionized water, then beaker proceeds to digital display tests the speed constant temperature blender with magnetic force
In, it is 88 DEG C in temperature, under the conditions of rotating speed is 450r/min, constant temperature stirs until solid is completely dissolved, and obtains mixed solution；Finally
Count by weight, take 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 successively
Acid ammonium, adds taken mixed solution, Ammonium persulfate. and deionized water in reactor, is 78 DEG C in temperature, and rotating speed is 500r/
Under the conditions of min, constant temperature stirring mixing 5min, under constant temperature stirring, drip taken vinyl acetate, controlling time for adding is
70min, continues constant temperature stirring reaction 7h, and reaction terminates, and stands, naturally cools to room temperature, obtain white emulsion, be weather resistant tough
Property white glue with vinyl.
The weather resistant toughness white glue with vinyl that the present invention is prepared be used for ceramic tile and cement wall () stickup in face, in mass ratio 1:
3, white glue with vinyl is mixed with tap water and mixes well, prepare mixture, mixture is mixed into pasty state glue with cement 1:5 in mass ratio,
Pasty state sol is scraped in cement wall () on face, then the ceramic tile that need to paste is pressed on coated face.This white glue with vinyl weatherability
Good with resistance to impact, under the conditions of-5 DEG C, freezing 27h, occurs without freezeout, and shear strength reaches 3.57MPa, and viscosity is
12.9Pa s, at 25 DEG C, adhesive strength is 92MPa, is worthy to be popularized and uses.
Example 3
First weigh Fresh Laminaria Japonica 500g, through manually shredding into 3 × 3cm fragment, then the addition of gained fragment is filled 3L deionization
In the cast iron pan of water, heated and boiled 15min, filtered while hot, proceed to filtration gained Thallus Laminariae (Thallus Eckloniae) fragment subsequently stone grinder grinds
20min, is mixed into 2L deionized water in process of lapping, collects to obtain Thallus Laminariae (Thallus Eckloniae) serosity；Measure 1000mL above-mentioned gained Thallus Laminariae (Thallus Eckloniae) serosity, add
Enter to fill in the fermentation tank of 400mL deionized water, add 100g second pond activated sludge, open fermenter stirrer, with
After 800r/min rotating speed stirring mixing 15min, in fermentation tank, it is passed through compressed air with 5mL/min speed, is 42 DEG C in temperature,
Under the conditions of rotating speed is 160r/min, ferment 36h, obtains mixed fermentation thing；Above-mentioned gained mixed fermentation thing is proceeded in steamer, in 95
Steaming and decocting 20min under the conditions of DEG C, proceeds to sonic oscillation instrument the most while hot, extracts 20min with 240W power ultrasonic, filters, and removes filter
Slag, obtains fermentation liquid, then is proceeded in Rotary Evaporators, under the conditions of temperature is 80 DEG C, and the 1/3 of concentrated by rotary evaporation to original volume,
Mucus must be concentrated；Measure the above-mentioned gained of 120mL the most successively and concentrate mucus, 10mL glacial acetic acid and 8mL acetic anhydride, add three mouthfuls of burnings
In Ping, then there-necked flask proceeded to digital display test the speed in constant temperature blender with magnetic force, adjust the temperature to 40 DEG C, rotating speed to 400r/min,
Under constant temperature stirring, dropping 5mL mass fraction is 98% sulphuric acid, waits to drip complete, is heated to 85 DEG C, insulated and stirred
Reaction 8h；Question response terminates, and is poured into by material in there-necked flask and fills in the beaker that 600mL temperature is 8 DEG C of cold water, uses Glass rod
Stirring mixing 5min, filters, removes filtrate, is washed with deionized by gained filter cake 5 times, filter cake proceeds to vacuum drying subsequently
In case, under the conditions of temperature is 70 DEG C, it is dried 8h, obtains buff white solid；Weigh successively 120g above-mentioned gained buff white solid and
120g polyvinyl alcohol, adds and fills in the beaker of 800mL deionized water, then beaker proceeds to digital display tests the speed constant temperature blender with magnetic force
In, it is 90 DEG C in temperature, under the conditions of rotating speed is 500r/min, constant temperature stirs until solid is completely dissolved, and obtains mixed solution；Finally
Count by weight, take 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 successively
Acid ammonium, adds taken mixed solution, Ammonium persulfate. and deionized water in reactor, is 80 DEG C in temperature, and rotating speed is 600r/
Under the conditions of min, constant temperature stirring mixing 6min, under constant temperature stirring, drip taken vinyl acetate, controlling time for adding is
80min, continues constant temperature stirring reaction 8h, and reaction terminates, and stands, naturally cools to room temperature, obtain white emulsion, be weather resistant tough
Property white glue with vinyl.
The weather resistant toughness white glue with vinyl that the present invention is prepared be used for ceramic tile and cement wall () stickup in face, in mass ratio 1:
3, white glue with vinyl is mixed with tap water and mixes well, prepare mixture, mixture is mixed into pasty state glue with cement 1:5 in mass ratio,
Pasty state sol is scraped in cement wall () on face, then the ceramic tile that need to paste is pressed on coated face.This white glue with vinyl weatherability
Good with resistance to impact, under the conditions of-4 DEG C, freezing 30h, occurs without freezeout, and shear strength reaches 3.86MPa, and viscosity is
13.2Pa s, at 25 DEG C, adhesive strength is 99MPa, is worthy to be popularized and uses.
Claims (1)
1. the preparation method of a weather resistant toughness white glue with vinyl, it is characterised in that concrete preparation process is:
(1) weigh Fresh Laminaria Japonica 300～500g, through manually shredding into 3 × 3cm fragment, then the addition of gained fragment is filled 2～3L
In the cast iron pan of deionized water, heated and boiled 10～15min, filtered while hot, subsequently filtration gained Thallus Laminariae (Thallus Eckloniae) fragment is proceeded to stone grinder
Middle grinding 15～20min, is mixed into 1～2L deionized water in process of lapping, collects to obtain Thallus Laminariae (Thallus Eckloniae) serosity；
(2) measure 800～1000mL above-mentioned gained Thallus Laminariae (Thallus Eckloniae) serosity, add in the fermentation tank filling 300～400mL deionized waters,
Add 80～100g second pond activated sludge, open fermenter stirrer, with 600～800r/min rotating speeds stirring mixing 10～
After 15min, in fermentation tank, be passed through compressed air with 3～5mL/min speed, be 40～42 DEG C in temperature, rotating speed be 120～
Under the conditions of 160r/min, fermentation 24～36h, obtain mixed fermentation thing；
(3) above-mentioned gained mixed fermentation thing is proceeded in steamer, steaming and decocting 15～20min under the conditions of 90～95 DEG C, the most while hot
Proceed to sonic oscillation instrument, extract 15～20min with 200～240W power ultrasonics, filter, remove filtering residue, obtain fermentation liquid, then by it
Proceed 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) measure 100～120mL above-mentioned gained successively and concentrate mucus, 8～10mL glacial acetic acid and 6～8mL acetic anhydride, add three
In mouthful flask, then there-necked flask proceeds to digital display testing the speed in constant temperature blender with magnetic force, adjust the temperature to 35～40 DEG C, rotating speed is extremely
350～400r/min, under constant temperature stirring, dropping 3～5mL mass fractions are 98% sulphuric acid, wait to drip complete, and heating rises
Temperature is to 80～85 DEG C, and insulated and stirred reacts 6～8h；
(5) question response terminates, and is poured into by material in there-necked flask and fills in the beaker that 500～600mL temperature are 6～8 DEG C of cold water,
With Glass rod stirring mixing 3～5min, filter, remove filtrate, gained filter cake is washed with deionized 3～5 times, subsequently will filter
Cake proceeds in vacuum drying oven, is dried 6～8h, obtains buff white solid under the conditions of temperature is 65～70 DEG C；
(6) weigh 100～120g above-mentioned gained buff white solid and 100～120g polyvinyl alcohol successively, add fill 600～
In the beaker of 800mL deionized water, then beaker proceeded to digital display test the speed in constant temperature blender with magnetic force, be 85～90 DEG C in temperature,
Under the conditions of rotating speed is 400～500r/min, constant temperature stirs until solid is completely dissolved, and obtains mixed solution；
(7) count by weight, take 45～50 parts of vinyl acetates, 25～30 parts of above-mentioned gained mixed solutions, 180～200 successively
Part deionized water and 0.5～0.8 part of Ammonium persulfate., add taken mixed solution, Ammonium persulfate. and deionized water in reactor,
Being 75～80 DEG C in temperature, under the conditions of rotating speed is 400～600r/min, constant temperature stirring mixing 4～6min, at constant temperature stirring
Under, drip taken vinyl acetate, controlling time for adding is 60～80min, continues constant temperature stirring reaction 6～8h, and reaction terminates, quiet
Put, naturally cool to room temperature, obtain white emulsion, be weather resistant toughness white glue with vinyl.
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| CN110368022A (en) * | 2019-07-23 | 2019-10-25 | 上海市嘉定区中心医院 | A kind of coupling device for ultrasound detection head |
| CN111823336A (en) * | 2020-07-28 | 2020-10-27 | 三棵树涂料股份有限公司 | Aldehyde-free technical veneer production method for veneer solid wood multilayer board assembly |
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