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CN108384503A - A kind of preparation method of the special adhesive of flexible face brick - Google Patents

A kind of preparation method of the special adhesive of flexible face brick Download PDF

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CN108384503A
CN108384503A CN201810137269.2A CN201810137269A CN108384503A CN 108384503 A CN108384503 A CN 108384503A CN 201810137269 A CN201810137269 A CN 201810137269A CN 108384503 A CN108384503 A CN 108384503A
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stirred
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张芸
殷连海
张淼
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04Polyurethanes
    • C09J175/06Polyurethanes from polyesters
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08Processes
    • C08G18/0804Manufacture of polymers containing ionic or ionogenic groups
    • C08G18/0819Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups
    • C08G18/0823Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups containing carboxylate salt groups or groups forming them
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30Low-molecular-weight compounds
    • C08G18/32Polyhydroxy compounds; Polyamines; Hydroxyamines
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    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30Low-molecular-weight compounds
    • C08G18/34Carboxylic acids; Esters thereof with monohydroxyl compounds
    • C08G18/348Hydroxycarboxylic acids
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30Low-molecular-weight compounds
    • C08G18/36Hydroxylated esters of higher fatty acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/42Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/4266Polycondensates having carboxylic or carbonic ester groups in the main chain prepared from hydroxycarboxylic acids and/or lactones
    • C08G18/4269Lactones
    • C08G18/4277Caprolactone and/or substituted caprolactone
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/67Unsaturated compounds having active hydrogen
    • C08G18/671Unsaturated compounds having only one group containing active hydrogen
    • C08G18/672Esters of acrylic or alkyl acrylic acid having only one group containing active hydrogen
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72Polyisocyanates or polyisothiocyanates
    • C08G18/74Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/75Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
    • C08G18/751Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Polyurethanes Or Polyureas (AREA)

Abstract

The invention discloses a kind of preparation methods of the special adhesive of flexible face brick, belong to adhesive technical field.Polycaprolactone glycol and trimethylhexane diisocyanate constant temperature are stirred to react by the present invention, cooling, and N methyl pyrrolidones are added and are stirred to react, dihydromethyl propionic acid is then added, trimethylolpropane, ethylene glycol, butanediol, cottonseed oil, dibutyl tin laurate constant temperature is stirred to react, and is subsequently added into acrylic acid hydrocarbon ethyl ester and is stirred to react, cooling, triethylene tetramine is added and deionized water is stirred to get modified polyurethane emulsion;Polyacrylamide resin and ion water termostat are stirred, surfactant is added and chromium trichloride solution constant temperature is stirred to get modified emulsion;By modified polyurethane emulsion, modified emulsion, modified filler, silane coupling agent and carbomer are stirred to get the special adhesive of flexible face brick.The special adhesive of flexible face brick provided by the invention has excellent flexibility and adhesion strength.

Description

A kind of preparation method of the special adhesive of flexible face brick
Technical field
The invention discloses a kind of preparation methods of the special adhesive of flexible face brick, belong to adhesive technical field.
Background technology
As modern people's living standard improves, the improvement of living conditions is advocated in country under building energy conservation emission reduction policy It needs and a kind of meeting low-carbon environment-friendly, multi-functional, decorative strong building and ornament materials to replace original traditional organic dress The high energy consumptions material such as plaque, glass curtain wall, coating, ceramic tile and stone material.
Multi-use architecture energy-saving flexible ornament materials building decorations patch(Porcelain tendre)It is to be modified common inorganic powder, then to be modified nothing Machine powder is made of main component, has not only remained the resistance to ag(e)ing of inorganic material, but also the flexibility with organic material.Porcelain tendre, and Non-real porcelain, nor ceramic tile, it is a kind of novel building and ornament materials.According to《Porcelain tendre building decoration engineering technology is advised Journey》It explains:By modified soil(MCM)For primary raw material, with special temperature control moulding system molding, baking, cross-linking radiation and At one kind have building decoration plane materiel flexible.At the beginning of birth, it has the appearance of ceramic tile, therefore is commonly called as soft Porcelain with the development of technology, can develop to imitative stone material, leather texture imitation, imitation wood etc. later, and every to imagine, porcelain tendre is all It can be achieved.
The coefficient of thermal expansion of different materials is different, and on combined two kinds of material interfaces, the sufficiently large temperature difference can Larger shear stress can be caused to interface, influence the fastness of material combination.It, on the one hand should be as possible to reduce warm and humid shear stress Selection line the is swollen small combination of materials of difference of coefficients, another aspect, it is also necessary to consider the flexibility index of binding material.Porcelain tendre is flexible Face brick is starched using dedicated bonding, and main component is mud powder and acrylic emulsions.But porcelain tendre adhesive traditional at present There is a problem of that flexibility and adhesion strength are bad, therefore also needs to study it.
Invention content
The present invention solves the technical problem of:It is asked for traditional soft porcelain adhesive flexibility and adhesion strength are bad Topic, provides a kind of preparation method of the special adhesive of flexible face brick.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
(1)It counts in parts by weight, takes 20~30 parts of polycaprolactone glycols successively, 40~50 parts of trimethylhexane diisocyanates, 2 ~3 parts of N-Methyl pyrrolidones, 3~5 parts of dihydromethyl propionic acids, 3~5 parts of trimethylolpropanes, 2~3 parts of ethylene glycol, 2~3 parts Butanediol, 5~8 portions of cottonseed oils, 1~2 part of dibutyl tin laurate, 3~5 parts of acrylic acid hydrocarbon ethyl esters, 3~5 parts of triethylenes four Amine, 60~80 parts of deionized waters, polycaprolactone glycol and trimethylhexane diisocyanate constant temperature are stirred to react, and cooling adds Enter N-Methyl pyrrolidone to be stirred to react, dihydromethyl propionic acid, trimethylolpropane, ethylene glycol, butanediol, cottonseed is then added Oil, dibutyl tin laurate constant temperature are stirred to react, and are subsequently added into acrylic acid hydrocarbon ethyl ester and are stirred to react, and triethylene is added in cooling Tetramine and deionized water are stirred to get modified polyurethane emulsion;
(2)It counts in parts by weight, takes 20~30 parts of polyacrylamide resins, 60~80 parts of deionized waters, 8~10 parts of surfaces successively Activating agent, 5~10 parts of chromium trichloride solution, polyacrylamide resin and ion water termostat are stirred, and add surface work Property agent and chromium trichloride solution constant temperature are stirred to get modified emulsion;
(3)It counts in parts by weight, by 60~80 parts of modified polyurethane emulsions, 80~100 parts of modified emulsions, 30~40 parts of modifications are filled out Material, 8~10 parts of silane coupling agents and 8~10 parts of carbomers are stirred to get the special adhesive of flexible face brick.
Step(2)The surfactant is Tween-85, any one in Si Pan -60 or Si Pan -80.
Step(3)The preparation process of the modified filler is:By sepiolite ball mill grinding, sieving obtains sepiolite powder, will be extra large Afrodite powder and hydrochloric acid in mass ratio 1:50~1:100 are stirred reaction, filter, washing, dry to get modified filler.
Step(3)The silane coupling agent is silane resin acceptor kh-550, silane coupling agent KH-560 or silane coupling agent Any one in KH-570.
Step(3)The carbomer is carbomer 930, any one in carbomer 937 or Acritamer 940.
The beneficial effects of the invention are as follows:
(1)The present invention contains a large amount of double bond and carboxyl-functional by adding modified polyurethane emulsion in cotton seed oil minor structure Group, after being added in polyurethane resin systems so that polyurethane resin molecular chain-end double bond content increases, and resin is in solidification process In, terminal double bond reaction compartment steric hindrance is smaller, while with the presence of carboxyl isopolarity functional group, emulsion particle cohesive force can be made to obtain Enhancing further promotes product adhesion strength, meanwhile, the aliphatic long-chain structure in cottonseed oil molecule can effectively promote system Flexibility and shock resistance;
(2)The present invention is by adding modified emulsion, and first, during emulsion modified, trivalent chromic ion promotes as crosslinking agent Micro- crosslinking occurs inside system, forms micro- cross-linked network, during storage, due to the presence of micro- cross-linking system, plays good Good thickening effect, avoids system from being separated, the stability of emulsion system is effectively ensured, to effectively promote the storage of product Stability is deposited, secondly, in use, since trivalent chromic ion cross-linking system gel-formation power is stronger, is added in system, makes Between colloid cohesive force increase, to promote the adhesion strength of product, again, when the external world is there are when the larger temperature difference, the larger temperature difference So that gluing interface goes out there are larger shear stress, since trivalent chromic ion cross-linking system has good viscoplasticity, when There are when shear stress effect, system can be restored system automatically, and shear stress is avoided to cause harmful effect to cross-linking system, to effectively Promote the adhesion strength of product.
Specific implementation mode
Sepiolite is placed in ball mill grinding in ball mill, the sieve of 200~300 mesh is crossed, obtains sepiolite powder, by sepiolite powder with The hydrochloric acid in mass ratio 1 that mass fraction is 20~30%:50~1:100 are placed in single-necked flask, in rotating speed be 300~500r/ Under the conditions of min, it is stirred 30~50min of reaction, mixed liquor is obtained, then mixed liquor is filtered, obtains filter residue, then spend filter residue Filter residue after washing, is then placed in baking oven by ion water washing 3~5 times, and under the conditions of temperature is 105~110 DEG C, drying is extremely Constant weight is to get modified filler;It counts in parts by weight, takes 20~30 parts of polycaprolactone glycols, 40~50 parts of trimethyl cyclohexanes successively Diisocyanate, 2~3 parts of N-Methyl pyrrolidones, 3~5 parts of dihydromethyl propionic acids, 3~5 parts of trimethylolpropanes, 2~3 parts Ethylene glycol, 2~3 parts of butanediols, 5~8 portions of cottonseed oils, 1~2 part of dibutyl tin laurate, 3~5 parts of acrylic acid hydrocarbon ethyl esters, 3 ~5 parts of triethylene tetramines, 60~80 parts of deionized waters, are first placed in three by polycaprolactone glycol and trimethylhexane diisocyanate In mouthful flask, and three-necked flask is placed in digital display and is tested the speed in constant temperature blender with magnetic force, in temperature be 85~95 DEG C, rotating speed 300 Under the conditions of~500r/min, constant temperature is stirred to react 1~2h, and the temperature in three-necked flask is then down to 70~75 DEG C, then to three N-Methyl pyrrolidone is added in mouth flask, under the conditions of rotating speed is 300~500r/min, is stirred to react 20~30min, then Dihydromethyl propionic acid, trimethylolpropane, ethylene glycol, butanediol, two fourth of cottonseed oil and tin dilaurate are added into three-necked flask Ji Xi is 70~75 DEG C in temperature, and under the conditions of rotating speed is 300~500r/min, constant temperature is stirred to react 3~4h, then to three mouthfuls Acrylic acid hydrocarbon ethyl ester is added in flask, is 70~75 DEG C in temperature, under the conditions of rotating speed is 300~500r/min, is stirred to react 30 ~50min, then temperature in three-necked flask is down to 30~35 DEG C, triethylene tetramine and deionization are then added into three-necked flask Water is stirred 30~50min to get modified polyurethane emulsion under the conditions of rotating speed is 300~500r/min;By weight Number meter, takes 20~30 parts of polyacrylamide resins successively, 60~80 parts of deionized waters, 8~10 parts of surfactants, 5~10 parts Mass concentration is the chromium trichloride solution of 150~200mg/L, and first polyacrylamide resin and ionized water are placed in beaker, and Beaker is placed in digital display to test the speed in constant temperature blender with magnetic force, is 55~65 DEG C in temperature, rotating speed is 300~500r/min conditions Under, constant temperature is stirred 30~50min, then surfactant and mass concentration is added as the three of 150~200mg/L into beaker Chromium chloride solution, in 55~65 DEG C, under the conditions of rotating speed is 3000~4500r/min, constant temperature high-speed stirred mixes 40~60min, Up to modified emulsion;It counts in parts by weight, by 60~80 parts of modified polyurethane emulsions, 80~100 parts of modified emulsions, 30~40 parts Modified filler, 8~10 parts of silane coupling agents and 8~10 parts of carbomers are placed in batch mixer, in rotating speed be 1200~1300r/min Under the conditions of, 40~60min is stirred to get the special adhesive of flexible face brick.
Example 1
Sepiolite is placed in ball mill grinding in ball mill, the sieve of 300 mesh is crossed, sepiolite powder is obtained, by sepiolite powder and mass fraction For 30% hydrochloric acid in mass ratio 1:100 are placed in single-necked flask, under the conditions of rotating speed is 500r/min, are stirred reaction 50min obtains mixed liquor, then mixed liquor is filtered, and obtains filter residue, and then filter residue is washed with deionized 5 times, after then washing Filter residue be placed in baking oven, under the conditions of temperature is 110 DEG C, it is dry to constant weight to get modified filler;It counts in parts by weight, according to It is secondary to take 30 parts of polycaprolactone glycols, 50 parts of trimethylhexane diisocyanates, 3 parts of N-Methyl pyrrolidones, 5 parts of dihydroxymethyls third Acid, 5 parts of trimethylolpropanes, 3 parts of ethylene glycol, 3 parts of butanediols, 8 portions of cottonseed oils, 2 parts of dibutyl tin laurates, 5 parts of propylene Sour hydrocarbon ethyl ester, 5 parts of triethylene tetramines, 80 parts of deionized waters first set polycaprolactone glycol and trimethylhexane diisocyanate In three-necked flask, and three-necked flask is placed in digital display and is tested the speed in constant temperature blender with magnetic force, is 95 DEG C in temperature, rotating speed is Under the conditions of 500r/min, constant temperature is stirred to react 2h, the temperature in three-necked flask is then down to 75 DEG C, then add into three-necked flask Enter N-Methyl pyrrolidone, under the conditions of rotating speed is 500r/min, 30min is stirred to react, then to being added two in three-necked flask Hydroxymethyl propionic acid, trimethylolpropane, ethylene glycol, butanediol, cottonseed oil and dibutyl tin laurate, in temperature be 75 DEG C, Under the conditions of rotating speed is 500r/min, constant temperature is stirred to react 4h, and acrylic acid hydrocarbon ethyl ester is then added into three-necked flask, is in temperature 75 DEG C, under the conditions of rotating speed is 500r/min, it is stirred to react 50min, then temperature in three-necked flask is down to 35 DEG C, then to three mouthfuls Triethylene tetramine and deionized water are added in flask, under the conditions of rotating speed is 500r/min, is stirred 50min to get modification Polyaminoester emulsion;It counts in parts by weight, takes 30 parts of polyacrylamide resins successively, 80 parts of deionized waters, 10 parts of surfactants, Polyacrylamide resin and ionized water, are first placed in beaker by the chromium trichloride solution that 10 parts of mass concentrations are 200mg/L, and will Beaker is placed in digital display and tests the speed in constant temperature blender with magnetic force, is 65 DEG C in temperature, under the conditions of rotating speed is 500r/min, constant temperature stirring is mixed 50min is closed, then the chromium trichloride solution that surfactant and mass concentration are 200mg/L is added into beaker, in 65 DEG C, rotating speed Under the conditions of 4500r/min, constant temperature high-speed stirred mixes 60min to get modified emulsion;It counts in parts by weight, by 80 parts of modifications Polyaminoester emulsion, 100 parts of modified emulsions, 40 parts of modified fillers, 10 parts of silane coupling agents and 10 parts of carbomers are placed in batch mixer, Under the conditions of rotating speed is 1300r/min, 60min is stirred to get the special adhesive of flexible face brick.
Example 2
It counts in parts by weight, takes 30 parts of polycaprolactone glycols, 50 parts of trimethylhexane diisocyanates, 3 parts of N- methyl pyrroles successively Pyrrolidone, 5 parts of dihydromethyl propionic acids, 5 parts of trimethylolpropanes, 3 parts of ethylene glycol, 3 parts of butanediols, 2 parts of di lauric dibutyls Tin, 5 parts of acrylic acid hydrocarbon ethyl esters, 5 parts of triethylene tetramines, 80 parts of deionized waters, first by polycaprolactone glycol and trimethyl cyclohexane two Isocyanates is placed in three-necked flask, and three-necked flask is placed in digital display and is tested the speed in constant temperature blender with magnetic force, in temperature be 95 DEG C, Under the conditions of rotating speed is 500r/min, constant temperature is stirred to react 2h, the temperature in three-necked flask is then down to 75 DEG C, then burn to three mouthfuls N-Methyl pyrrolidone is added in bottle, under the conditions of rotating speed is 500r/min, 30min is stirred to react, then in three-necked flask Dihydromethyl propionic acid, trimethylolpropane, ethylene glycol, butanediol and dibutyl tin laurate is added, is 75 DEG C in temperature, turns Speed be 500r/min under the conditions of, constant temperature is stirred to react 4h, then into three-necked flask be added acrylic acid hydrocarbon ethyl ester, in temperature be 75 DEG C, under the conditions of rotating speed is 500r/min, it is stirred to react 50min, then temperature in three-necked flask is down to 35 DEG C, is then burnt to three mouthfuls Triethylene tetramine and deionized water are added in bottle, under the conditions of rotating speed is 500r/min, is stirred 50min to get flexible face The special adhesive of brick.
Example 3
Sepiolite is placed in ball mill grinding in ball mill, the sieve of 300 mesh is crossed, sepiolite powder is obtained, by sepiolite powder and mass fraction For 30% hydrochloric acid in mass ratio 1:100 are placed in single-necked flask, under the conditions of rotating speed is 500r/min, are stirred reaction 50min obtains mixed liquor, then mixed liquor is filtered, and obtains filter residue, and then filter residue is washed with deionized 5 times, after then washing Filter residue be placed in baking oven, under the conditions of temperature is 110 DEG C, it is dry to constant weight to get modified filler;It counts in parts by weight, according to It is secondary to take 30 parts of polycaprolactone glycols, 50 parts of trimethylhexane diisocyanates, 3 parts of N-Methyl pyrrolidones, 5 parts of dihydroxymethyls third Acid, 5 parts of trimethylolpropanes, 3 parts of ethylene glycol, 3 parts of butanediols, 2 parts of dibutyl tin laurates, 5 parts of acrylic acid hydrocarbon ethyl esters, 5 Polycaprolactone glycol and trimethylhexane diisocyanate are first placed in three-necked flask by part triethylene tetramine, 80 parts of deionized waters In, and three-necked flask is placed in digital display and is tested the speed in constant temperature blender with magnetic force, it is 95 DEG C in temperature, rotating speed is 500r/min conditions Under, constant temperature is stirred to react 2h, the temperature in three-necked flask is then down to 75 DEG C, then N- methylpyrroles are added into three-necked flask Alkanone is stirred to react 30min under the conditions of rotating speed is 500r/min, then to being added dihydromethyl propionic acid in three-necked flask, three Hydroxymethyl-propane, ethylene glycol, butanediol and dibutyl tin laurate, in temperature be 75 DEG C, rotating speed be 500r/min under the conditions of, Constant temperature is stirred to react 4h, and acrylic acid hydrocarbon ethyl ester is then added into three-necked flask, is 75 DEG C in temperature, rotating speed is 500r/min items Under part, it is stirred to react 50min, then temperature in three-necked flask is down to 35 DEG C, triethylene tetramine is then added into three-necked flask And deionized water is stirred 50min to get modified polyurethane emulsion under the conditions of rotating speed is 500r/min;In parts by weight Meter takes 30 parts of polyacrylamide resins successively, and 80 parts of deionized waters, 10 parts of surfactants, 10 parts of mass concentrations are 200mg/L Chromium trichloride solution, first polyacrylamide resin and ionized water are placed in beaker, and beaker is placed in digital display and is tested the speed constant temperature It it is 65 DEG C in temperature, under the conditions of rotating speed is 500r/min, constant temperature is stirred 50min, then adds into beaker in magnetic stirring apparatus Enter the chromium trichloride solution that surfactant and mass concentration are 200mg/L, it is permanent under the conditions of rotating speed is 4500r/min in 65 DEG C Warm high-speed stirred mixes 60min to get modified emulsion;It counts in parts by weight, by 80 parts of modified polyurethane emulsions, 100 parts of modifications Lotion, 40 parts of modified fillers, 10 parts of silane coupling agents and 10 parts of carbomers are placed in batch mixer, in rotating speed be 1300r/min items Under part, 60min is stirred to get the special adhesive of flexible face brick.
Example 4
Sepiolite is placed in ball mill grinding in ball mill, the sieve of 300 mesh is crossed, sepiolite powder is obtained, by sepiolite powder and mass fraction For 30% hydrochloric acid in mass ratio 1:100 are placed in single-necked flask, under the conditions of rotating speed is 500r/min, are stirred reaction 50min obtains mixed liquor, then mixed liquor is filtered, and obtains filter residue, and then filter residue is washed with deionized 5 times, after then washing Filter residue be placed in baking oven, under the conditions of temperature is 110 DEG C, it is dry to constant weight to get modified filler;It counts in parts by weight, according to It is secondary to take 30 parts of polycaprolactone glycols, 50 parts of trimethylhexane diisocyanates, 3 parts of N-Methyl pyrrolidones, 5 parts of dihydroxymethyls third Acid, 5 parts of trimethylolpropanes, 3 parts of ethylene glycol, 3 parts of butanediols, 8 portions of cottonseed oils, 2 parts of dibutyl tin laurates, 5 parts of propylene Sour hydrocarbon ethyl ester, 5 parts of triethylene tetramines, 80 parts of deionized waters first set polycaprolactone glycol and trimethylhexane diisocyanate In three-necked flask, and three-necked flask is placed in digital display and is tested the speed in constant temperature blender with magnetic force, is 95 DEG C in temperature, rotating speed is Under the conditions of 500r/min, constant temperature is stirred to react 2h, the temperature in three-necked flask is then down to 75 DEG C, then add into three-necked flask Enter N-Methyl pyrrolidone, under the conditions of rotating speed is 500r/min, 30min is stirred to react, then to being added two in three-necked flask Hydroxymethyl propionic acid, trimethylolpropane, ethylene glycol, butanediol, cottonseed oil and dibutyl tin laurate, in temperature be 75 DEG C, Under the conditions of rotating speed is 500r/min, constant temperature is stirred to react 4h, and acrylic acid hydrocarbon ethyl ester is then added into three-necked flask, is in temperature 75 DEG C, under the conditions of rotating speed is 500r/min, it is stirred to react 50min, then temperature in three-necked flask is down to 35 DEG C, then to three mouthfuls Triethylene tetramine and deionized water are added in flask, under the conditions of rotating speed is 500r/min, is stirred 50min to get modification Polyaminoester emulsion;It counts in parts by weight, by 80 parts of modified polyurethane emulsions, 40 parts of modified fillers, 10 parts of silane coupling agents and 10 Part carbomer is placed in batch mixer, under the conditions of rotating speed is 1300r/min, is stirred 60min to get flexible face brick special glue Glutinous agent.
Example 5
It counts in parts by weight, takes 30 parts of polycaprolactone glycols, 50 parts of trimethylhexane diisocyanates, 3 parts of N- methyl pyrroles successively Pyrrolidone, 5 parts of dihydromethyl propionic acids, 5 parts of trimethylolpropanes, 3 parts of ethylene glycol, 3 parts of butanediols, 8 portions of cottonseed oils, 2 parts of February Dilaurylate, 5 parts of acrylic acid hydrocarbon ethyl esters, 5 parts of triethylene tetramines, 80 parts of deionized waters, first by polycaprolactone glycol and three Methyl hexane diisocyanate is placed in three-necked flask, and three-necked flask is placed in digital display and is tested the speed in constant temperature blender with magnetic force, in Temperature is 95 DEG C, and under the conditions of rotating speed is 500r/min, constant temperature is stirred to react 2h, and the temperature in three-necked flask is then down to 75 DEG C, then N-Methyl pyrrolidone is added into three-necked flask, under the conditions of rotating speed is 500r/min, it is stirred to react 30min, then Dihydromethyl propionic acid, trimethylolpropane, ethylene glycol, butanediol, two fourth of cottonseed oil and tin dilaurate are added into three-necked flask Ji Xi is 75 DEG C in temperature, and under the conditions of rotating speed is 500r/min, constant temperature is stirred to react 4h, and third is then added into three-necked flask Olefin(e) acid hydrocarbon ethyl ester is 75 DEG C in temperature, under the conditions of rotating speed is 500r/min, is stirred to react 50min, then by temperature in three-necked flask 35 DEG C are down to, triethylene tetramine and deionized water are then added into three-necked flask, under the conditions of rotating speed is 500r/min, stirring 50min is mixed to get modified polyurethane emulsion;It counts in parts by weight, takes 30 parts of polyacrylamide resins, 80 parts of deionizations successively Water, 10 parts of surfactants, 10 parts of mass concentrations are the chromium trichloride solution of 200mg/L, first by polyacrylamide resin and from Sub- water is placed in beaker, and beaker is placed in digital display and is tested the speed in constant temperature blender with magnetic force, in temperature be 65 DEG C, rotating speed 500r/ Under the conditions of min, constant temperature is stirred 50min, then surfactant and mass concentration is added as the trichlorine of 200mg/L into beaker Change chromium solution, in 65 DEG C, under the conditions of rotating speed is 4500r/min, constant temperature high-speed stirred mixes 60min to get modified emulsion;By weight Number meter is measured, by 80 parts of modified polyurethane emulsions, 100 parts of modified emulsions, 10 parts of silane coupling agents and 10 parts of carbomers are placed in mixed In material machine, under the conditions of rotating speed is 1300r/min, 60min is stirred to get the special adhesive of flexible face brick.
The special adhesive of 1 to 5 gained flexible face brick of example is subjected to performance detection, specific testing result is as shown in table 1:
Table 1:Performance detection table
Detection content Example 1 Example 2 Example 3 Example 4 Example 5
Backfin ratio/% 1.04 1.97 1.53 1.46 1.51
Adhesion strength/MPa 1.38 0.84 1.11 1.05 1.09
By 1 testing result of table it is found that the special adhesive effect of 2 gained flexible face brick of example is worst, present invention gained flexible face brick Special adhesive has excellent flexibility and adhesion strength.

Claims (5)

1. a kind of preparation method of the special adhesive of flexible face brick, it is characterised in that specific preparation process is as follows:
(1)It counts in parts by weight, takes 20~30 parts of polycaprolactone glycols successively, 40~50 parts of trimethylhexane diisocyanates, 2 ~3 parts of N-Methyl pyrrolidones, 3~5 parts of dihydromethyl propionic acids, 3~5 parts of trimethylolpropanes, 2~3 parts of ethylene glycol, 2~3 parts Butanediol, 5~8 portions of cottonseed oils, 1~2 part of dibutyl tin laurate, 3~5 parts of acrylic acid hydrocarbon ethyl esters, 3~5 parts of triethylenes four Amine, 60~80 parts of deionized waters, polycaprolactone glycol and trimethylhexane diisocyanate constant temperature are stirred to react, and cooling adds Enter N-Methyl pyrrolidone to be stirred to react, dihydromethyl propionic acid, trimethylolpropane, ethylene glycol, butanediol, cottonseed is then added Oil, dibutyl tin laurate constant temperature are stirred to react, and are subsequently added into acrylic acid hydrocarbon ethyl ester and are stirred to react, and triethylene is added in cooling Tetramine and deionized water are stirred to get modified polyurethane emulsion;
(2)It counts in parts by weight, takes 20~30 parts of polyacrylamide resins, 60~80 parts of deionized waters, 8~10 parts of surfaces successively Activating agent, 5~10 parts of chromium trichloride solution, polyacrylamide resin and ion water termostat are stirred, and add surface work Property agent and chromium trichloride solution constant temperature are stirred to get modified emulsion;
(3)It counts in parts by weight, by 60~80 parts of modified polyurethane emulsions, 80~100 parts of modified emulsions, 30~40 parts of modifications are filled out Material, 8~10 parts of silane coupling agents and 8~10 parts of carbomers are stirred to get the special adhesive of flexible face brick.
2. the preparation method of the special adhesive of a kind of flexible face brick according to claim 1, it is characterised in that:Step(2)Institute It is Tween-85 to state surfactant, any one in Si Pan -60 or Si Pan -80.
3. the preparation method of the special adhesive of a kind of flexible face brick according to claim 1, it is characterised in that:Step(3)Institute The preparation process for stating modified filler is:By sepiolite ball mill grinding, sieving obtains sepiolite powder, and sepiolite powder and hydrochloric acid are pressed matter Measure ratio 1:50~1:100 are stirred reaction, filter, washing, dry to get modified filler.
4. the preparation method of the special adhesive of a kind of flexible face brick according to claim 1, it is characterised in that:Step(3)Institute It is silane resin acceptor kh-550 to state silane coupling agent, any one in silane coupling agent KH-560 or Silane coupling reagent KH-570 Kind.
5. the preparation method of the special adhesive of a kind of flexible face brick according to claim 1, it is characterised in that:Step(3)Institute It is carbomer 930 to state carbomer, any one in carbomer 937 or Acritamer 940.
CN201810137269.2A 2018-02-10 2018-02-10 A kind of preparation method of the special adhesive of flexible face brick Withdrawn CN108384503A (en)

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Application publication date: 20180810