CN106866908B - A kind of preparation process of block of glass wool melamine modified phenolic resin - Google Patents
A kind of preparation process of block of glass wool melamine modified phenolic resin Download PDFInfo
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- CN106866908B CN106866908B CN201610760782.8A CN201610760782A CN106866908B CN 106866908 B CN106866908 B CN 106866908B CN 201610760782 A CN201610760782 A CN 201610760782A CN 106866908 B CN106866908 B CN 106866908B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/40—Chemically modified polycondensates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4833—Polyethers containing oxyethylene units
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6674—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
- C08G18/6677—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203 having at least three hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/675—Low-molecular-weight compounds
- C08G18/6755—Unsaturated carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/39—Aldehyde resins; Ketone resins; Polyacetals
- D06M15/423—Amino-aldehyde resins
Abstract
The present invention relates to a kind of preparation processes of block of glass wool melamine modified phenolic resin, belong to technical field of composite materials.Step：Modified polyurethane is prepared first, then prepares modified phenolic resin, and then phenol-formaldehyde resin modified, 300~600 parts of water, 5~10 parts of amphoteric surfactant, 3~7 parts of silane coupling agent, 5~10 parts of coupling agent, 2~4 parts of antioxidant are uniformly mixed, obtain immersion fluid；By 200~400 parts of block of glass wool, all infiltration is in immersion fluid, 20~take out be placed on partition board after forty minutes, after being flowed out there is no slurry, be placed in drying box, at a temperature of 30~80 DEG C will drying to get.By aqueous polyurethane and melamine, to phenolic resin modified, and then the size prepared for mineral wool is prepared in the present invention, and the thermal coefficient of the mineral wool produced is small, good corrosion resistance.
Description
Technical field
The present invention relates to a kind of preparation processes of block of glass wool melamine modified phenolic resin, belong to composite material skill
Art field.
Background technology
Mineral wool is while to add certain clinker to generate the silicate mineral of glass as primary raw material, through melting, at
Fibre simultaneously applies a certain amount of organic binder and manufactured cotton-like fiber simultaneously.With forming, bulk density is small, thermal conductivity
Go-to-and-fro, the advantage that heat preservation is adiabatic, sound absorption qualities are good, corrosion-resistant, stable chemical performance is good.Preparation method is by melten glass fiber
Change and be subject to the product that the formula binder of the environment-friendly type based on thermosetting resin is process, is that one kind only having several microns by diameter
The flexible felty body that is made of glass fibre, and can select different moisture proof pasters multiple online according to requirements
It closes.Its a large amount of small air void having, the effects that making it play insulation, sqouynd absorption lowering noise and security protection, be steel
Structural construction insulation, sqouynd absorption lowering noise optimal material.
Existing block of glass wool thermal coefficient as exterior-wall heat insulation is high, generally 0.042W/（m·K）, heat insulation effect is not
It is ideal, it is difficult to meet the requirement of 75% standard of building energy conservation；Heat-resisting quantity is relatively low, is 400 DEG C, using limited；And it is wanted to reach heat preservation
It asks, it is necessary to increase the thickness of block of glass wool, therefore increase difficulty of construction and construction cost.CN1962260A discloses a kind of environmental protection
Type formaldehyde-free glass wool, production technology are prepared by mineral wool raw material;High-temperature digestion, at fibre；Injection environment-friendly formaldehyde-free and
It is molded under glass wool adhesive condition of cure, the solidification temperature of mineral wool product is controlled at 100~300 DEG C in the production technology.
CN 104626666A disclose a kind of super layer structure extra-fine glass-wool felt, which is by the super of surface coated with resins binder
Thin centrifugal glass fibre interlayer heap poststack, forms through hot setting.The super layer structure extra-fine glass-wool felt fibre diameter is thin, and
Fibre diameter is in normal distribution, between layers close to parallel between the super layer structure for being 10 μm~100 μm, each layer
Cloth.CN 103571155A disclose a kind of blanket of glass wool and preparation method thereof.The blanket of glass wool is made of mineral wool, adhesive,
The adhesive includes：100 ~ 200 parts of resin, 150 ~ 250 parts of additive, 2 ~ 20 parts of blue colorant, softened water 160 ~
1100 parts.This adhesive is uniformly sprayed on mineral wool, cures 2 ~ 20min under 170 ~ 250 °C, you can at felt.
But the above-mentioned block of glass wool being prepared remains in use that thermal coefficient is excessive, corrosion resistance
Bad problem, is solved.
Invention content
The purpose of the present invention is：Solving block of glass wool, existing thermal coefficient is excessive in use, corrosion resistance is bad
Problem is mainly realized by being modified to the phenolic resin in preparation process.
Technical solution：
A kind of preparation process of block of glass wool melamine modified phenolic resin, includes the following steps：
1st step：By weight, the polyethylene glycol for taking 10~15 parts, the vacuum while stirring at a temperature of 100~110 DEG C
It is dehydrated 2~3h, is cooled to room temperature, 5~10 parts of toluene di-isocyanate(TDI), 2~4 parts of cationic monomer, maleic acid 2~4 is added
Part, 1~2 part of dibutyl tin laurate react 2~3h at 70~75 DEG C, 3~5 parts of glycerine are added, at 80~85 DEG C
20~60min of lower reaction, obtains modified polyurethane；
2nd step：By weight, catalyst is added in 60~80 parts of phenol, after heating, adds anion unsaturation
3~5 parts of 5~10 parts of monomer, 3~6 parts of lignin, 3~5 parts of urea and melamine, are reacted；
3rd step：In the reaction product that the 2nd step obtains, 50~70 parts of modified polyurethane and formaldehyde are added, is carried out anti-
It answers, after reaction, cooling discharge obtains phenol-formaldehyde resin modified；
4th step：By phenol-formaldehyde resin modified, 300~600 parts of water, 5~10 parts of amphoteric surfactant, silane coupling agent 3~
7 parts, 5~10 parts of coupling agent, 2~4 parts of antioxidant be uniformly mixed, obtain immersion fluid；
5th step：By 200~400 parts of block of glass wool, all infiltration is in immersion fluid, and 20~take out be placed in partition board after forty minutes
On, after there is no slurry flow out after, be placed in drying box in, at a temperature of 30~80 DEG C will drying to get.
In 1st step, cationic monomer is selected from MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, methacrylic acid two
Methylamino ethyl ester or dimethyl diallyl ammonium chloride.
In 2nd step, anion unsaturated monomer is selected from methacrylic acid, maleic acid, vinyl sulfonic acid, styrene sulphur
Acid, 2- (methyl) acrylamido -2- methyl propane sulfonic acids, 2- (methyl) acryloyl group ethane sulfonic acids and 2- (methyl) propylene
Propane sulfonic acid and their salt.
In 2nd step, between 40~50 DEG C of reaction temperature, 30~60min of reaction time.
In 2nd step, the lignin is bamboo acetic acid lignin, corncob alkali lignin, wheat stalk alkali
Any one or a few in lignin and poplar sulfate-reducing conditions.
In 2nd step, the catalyst is the mixture of sodium hydroxide and zinc oxide, sodium hydroxide and zinc oxide
Molar ratio is 1~1.5：1.
In 3rd step, between 90~95 DEG C of reaction temperature, 2~4h of reaction time.
In 4th step, coupling agent is silane coupling agent or titanate coupling agent.
In 4th step, amphoteric surfactant includes, for example, imidazolines surfactant, such as 2- hendecanes
Base-N, N- (hydroxyethyl carboxymethyl) -2- imidazolines sodium and 2- cocoyl -2- imidazoline hydroxylating -1- carboxy ethyl oxalic acid
Disodium (- 2-imidazoliniumhydroxyde-1-carboxyethyloxiate of disodium2-cocoyl)；Betaines
Surfactant, such as 2- heptadecyl-N- carboxymethyl group-N- hydroxyethyl imidazolines glycine betaines, lauryl dimethyl amino
Acetic acid glycine betaine, alkyl betaine, amido betaine and sulfobetaines；And amino acid surfactant, such as N- bays
Base glycine, N- lauryls-Beta-alanine and N- stearyls-Beta-alanine.
As antioxidant, such as triphenyl phosphite, three（4- aminomethyl phenyls）Phosphite ester, three（4- tert-butyl benzenes
Base）Phosphite ester, three（Single nonyl phenyl）Phosphite ester, three（2- methyl -4- ethylphenyls）Phosphite ester, three（2- methyl -4-
Tert-butyl-phenyl）Phosphite ester, three（2,4- di-t-butyl phenyl）Phosphite ester, three（2,6- di-t-butyl phenyl）Phosphorous acid
Ester, three（2,4- di-t-butyl -5- aminomethyl phenyls）Phosphite ester, three（It is single, dinonylphenyl）It is phosphite ester, double（Single nonyl benzene
Base）It is pentaerythrite-two-phosphite ester, double（2,4- di-t-butyl phenyl）It is pentaerythrite-two-phosphite ester, double（2,6- bis--
Tertiary butyl -4- aminomethyl phenyls）It is pentaerythrite-two-phosphite ester, double（Tri--tert-butyl-phenyls of 2,4,6-）Pentaerythrite-two-is sub-
It is phosphate, double（2,4- di-t-butyl -5- aminomethyl phenyls）Pentaerythrite-two-phosphite ester, 2,2- di-2-ethylhexylphosphine oxides（4,6- diformazans
Base phenyl）Octyl phosphite ester, 2,2- di-2-ethylhexylphosphine oxides（4- tertiary butyl -6- aminomethyl phenyls）Octyl phosphite ester, 2,2- methylene
It is double（4,6- di-t-butyl phenyl）Octyl phosphite ester, 2,2- di-2-ethylhexylphosphine oxides（4,6- 3,5-dimethylphenyls）Hexyl phosphite ester, 2,
2- di-2-ethylhexylphosphine oxides（4,6- 3,5-dimethylphenyls）Hexyl phosphite ester, 2,2- di-2-ethylhexylphosphine oxides（4,6- di-t-butyl phenyl）Stearyl
The bi-ester of phosphite such as phosphite ester；- four [3- of pentaerythrite base（3,5- di-t-butyl 4- hydroxy phenyls）Propionic ester], 1,
6- hexylene glycols-bis- [3-（3,5- di-t-butyl 4- hydroxy phenyls）Propionic ester], octadecyl -3-（3,5- di-t-butyl -4- hydroxyls
Base phenyl）Propionic ester, 1,3,5- trimethyls -2,4,6- three（3,5- di-t-butyl -4- hydroxyphenylmethyls）Benzene, triethylene glycol-are bis-
[3-（3- tertiary butyl -5- methyl -4- hydroxy phenyls）Propionic ester], the bis- { 2- [3- of 3,9-（3- tertiary butyl-4-hydroxy -5- methylbenzenes
Base）Propionyloxy] -1,1- dimethyl ethyls 2,4,8,10- tetra- oxaspiro [5,5] hendecane, [2- methyl-the 4- of 1,1,3- tri-
（3,5- di-t-butyl -4- hydroxy phenylpropionyl oxygroups）- 5- tert-butyl-phenyls] the fortified phenols class compound such as butane；5,7-
Di-t-butyl -3-（3,4- 3,5-dimethylphenyls）- 3H- benzofuran-2-ones etc..These can be used alone or two or more simultaneously
With.
Advantageous effect
The present invention, to phenolic resin modified, and then is prepared for glass cotton by aqueous polyurethane and melamine
The thermal coefficient of standby size, the mineral wool produced is small, good corrosion resistance.
Specific implementation mode
Embodiment 1
1st step：By weight, the polyethylene glycol for taking 10 parts, the vacuum dehydration 2h while stirring at a temperature of 100 DEG C are cold
But to room temperature, 5 parts of toluene di-isocyanate(TDI), 2 parts of cationic monomer MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, horse is added
Come sour 2 parts, 1 part of dibutyl tin laurate, react 2h at 70 DEG C, add 3 parts of glycerine, react 20min at 80 DEG C,
Obtain modified polyurethane；
2nd step：By weight, catalyst is added in 60 parts of phenol, and (catalyst is sodium hydroxide and zinc oxide mole
Than for 1~1 mixture), after heating, add 5 parts of anion unsaturated monomer styrene sulfonic acid, 3 parts of corncob alkali lignin,
3 parts of 3 parts of urea and melamine, are reacted, between 40 DEG C of reaction temperature, reaction time 30min；
3rd step：In the reaction product that the 2nd step obtains, 50 parts of modified polyurethane and formaldehyde are added, is reacted, instead
Between answering 90 DEG C of temperature, reaction time 2h, after reaction, cooling discharge obtains phenol-formaldehyde resin modified；
4th step：By phenol-formaldehyde resin modified, 300 parts of water, amphoteric surfactant lauryl dimethyl oxyneurine
5 parts, 3 parts of silane coupling agent, 5 parts of silane coupling agent, antioxidant it is double（2,4- di-t-butyl -5- aminomethyl phenyls）Pentaerythrite-
Two -2 parts of phosphite esters are uniformly mixed, and obtain immersion fluid；
5th step：Block of glass wool is all infiltrated in immersion fluid for 200 parts, takes out be placed on partition board after twenty minutes, wait for no longer
Have slurry outflow after, be placed in drying box in, at a temperature of 30 DEG C will drying to get.
Embodiment 2
1st step：By weight, the polyethylene glycol for taking 15 parts, the vacuum dehydration 3h while stirring at a temperature of 110 DEG C are cold
But to room temperature, be added 10 parts toluene di-isocyanate(TDI), 4 parts of cationic monomer MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride,
4 parts of maleic acid, 2 parts of dibutyl tin laurate, react 3h at 75 DEG C, add 5 parts of glycerine, are reacted at 85 DEG C
60min obtains modified polyurethane；
2nd step：By weight, catalyst is added in 80 parts of phenol, and (catalyst is sodium hydroxide and zinc oxide mole
Than for 1~1 mixture), after heating, add 10 parts of anion unsaturated monomer styrene sulfonic acid, corncob alkali lignin 6
5 parts of part, 5 parts of urea and melamine, are reacted, between 50 DEG C of reaction temperature, reaction time 60min；
3rd step：In the reaction product that the 2nd step obtains, 70 parts of modified polyurethane and formaldehyde are added, is reacted, instead
Between answering 95 DEG C of temperature, reaction time 4h, after reaction, cooling discharge obtains phenol-formaldehyde resin modified；
4th step：By phenol-formaldehyde resin modified, 600 parts of water, amphoteric surfactant lauryl dimethyl oxyneurine
5 parts, 3 parts of silane coupling agent, 5 parts of silane coupling agent, antioxidant it is double（2,4- di-t-butyl -5- aminomethyl phenyls）Pentaerythrite-
Two -2 parts of phosphite esters are uniformly mixed, and obtain immersion fluid；
5th step：Block of glass wool is all infiltrated in immersion fluid for 400 parts, takes out be placed on partition board after forty minutes, wait for no longer
Have slurry outflow after, be placed in drying box in, at a temperature of 80 DEG C will drying to get.
Embodiment 3
1st step：By weight, the polyethylene glycol for taking 12 parts, the vacuum dehydration 2h while stirring at a temperature of 105 DEG C are cold
But to room temperature, 6 parts of toluene di-isocyanate(TDI), 3 parts of cationic monomer MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, horse is added
Come sour 3 parts, 2 parts of dibutyl tin laurate, react 3h at 72 DEG C, add 4 parts of glycerine, react 40min at 82 DEG C,
Obtain modified polyurethane；
2nd step：By weight, catalyst is added in 70 parts of phenol, and (catalyst is sodium hydroxide and zinc oxide mole
Than for 1~1 mixture), after heating, add 7 parts of anion unsaturated monomer styrene sulfonic acid, 5 parts of corncob alkali lignin,
4 parts of 4 parts of urea and melamine, are reacted, between 45 DEG C of reaction temperature, reaction time 50min；
3rd step：In the reaction product that the 2nd step obtains, 60 parts of modified polyurethane and formaldehyde are added, is reacted, instead
Between answering 92 DEG C of temperature, reaction time 3h, after reaction, cooling discharge obtains phenol-formaldehyde resin modified；
4th step：By phenol-formaldehyde resin modified, 500 parts of water, amphoteric surfactant lauryl dimethyl oxyneurine
7 parts, 6 parts of silane coupling agent, 7 parts of silane coupling agent, antioxidant it is double（2,4- di-t-butyl -5- aminomethyl phenyls）Pentaerythrite-
Two -3 parts of phosphite esters are uniformly mixed, and obtain immersion fluid；
5th step：Block of glass wool is all infiltrated in immersion fluid for 300 parts, takes out and is placed on partition board after 30 minutes, waited for no longer
Have slurry outflow after, be placed in drying box in, at a temperature of 70 DEG C will drying to get.
Reference examples 1
With embodiment 3 difference lies in：Cationic monomer is not added in the preparation process of modified polyurethane.
1st step：By weight, the polyethylene glycol for taking 12 parts, the vacuum dehydration 2h while stirring at a temperature of 105 DEG C are cold
But to room temperature, 6 parts of toluene di-isocyanate(TDI), 3 parts of maleic acid, 2 parts of dibutyl tin laurate is added, is reacted at 72 DEG C
3h adds 4 parts of glycerine, reacts 40min at 82 DEG C, obtain modified polyurethane；
2nd step：By weight, catalyst is added in 70 parts of phenol, and (catalyst is sodium hydroxide and zinc oxide mole
Than for 1~1 mixture), after heating, add 7 parts of anion unsaturated monomer styrene sulfonic acid, 5 parts of corncob alkali lignin,
4 parts of 4 parts of urea and melamine, are reacted, between 45 DEG C of reaction temperature, reaction time 50min；
3rd step：In the reaction product that the 2nd step obtains, 60 parts of modified polyurethane and formaldehyde are added, is reacted, instead
Between answering 92 DEG C of temperature, reaction time 3h, after reaction, cooling discharge obtains phenol-formaldehyde resin modified；
4th step：By phenol-formaldehyde resin modified, 500 parts of water, amphoteric surfactant lauryl dimethyl oxyneurine
7 parts, 6 parts of silane coupling agent, 7 parts of silane coupling agent, antioxidant it is double（2,4- di-t-butyl -5- aminomethyl phenyls）Pentaerythrite-
Two -3 parts of phosphite esters are uniformly mixed, and obtain immersion fluid；
5th step：Block of glass wool is all infiltrated in immersion fluid for 300 parts, takes out and is placed on partition board after 30 minutes, waited for no longer
Have slurry outflow after, be placed in drying box in, at a temperature of 70 DEG C will drying to get.
Reference examples 2
With embodiment 3 difference lies in：Melamine is not added in 2nd step.
1st step：By weight, the polyethylene glycol for taking 12 parts, the vacuum dehydration 2h while stirring at a temperature of 105 DEG C are cold
But to room temperature, 6 parts of toluene di-isocyanate(TDI), 3 parts of cationic monomer MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, horse is added
Come sour 3 parts, 2 parts of dibutyl tin laurate, react 3h at 72 DEG C, add 4 parts of glycerine, react 40min at 82 DEG C,
Obtain modified polyurethane；
2nd step：By weight, catalyst is added in 70 parts of phenol, and (catalyst is sodium hydroxide and zinc oxide mole
Than for 1~1 mixture), after heating, add 7 parts of anion unsaturated monomer styrene sulfonic acid, 5 parts of corncob alkali lignin
With 4 parts of urea, reacted, between 45 DEG C of reaction temperature, reaction time 50min；
3rd step：In the reaction product that the 2nd step obtains, 60 parts of modified polyurethane and formaldehyde are added, is reacted, instead
Between answering 92 DEG C of temperature, reaction time 3h, after reaction, cooling discharge obtains phenol-formaldehyde resin modified；
4th step：By phenol-formaldehyde resin modified, 500 parts of water, amphoteric surfactant lauryl dimethyl oxyneurine
7 parts, 6 parts of silane coupling agent, 7 parts of silane coupling agent, antioxidant it is double（2,4- di-t-butyl -5- aminomethyl phenyls）Pentaerythrite-
Two -3 parts of phosphite esters are uniformly mixed, and obtain immersion fluid；
5th step：Block of glass wool is all infiltrated in immersion fluid for 300 parts, takes out and is placed on partition board after 30 minutes, waited for no longer
Have slurry outflow after, be placed in drying box in, at a temperature of 70 DEG C will drying to get.
Reference examples 3
With embodiment 3 difference lies in：Lignin is not added in 2nd step.
1st step：By weight, the polyethylene glycol for taking 12 parts, the vacuum dehydration 2h while stirring at a temperature of 105 DEG C are cold
But to room temperature, 6 parts of toluene di-isocyanate(TDI), 3 parts of cationic monomer MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, horse is added
Come sour 3 parts, 2 parts of dibutyl tin laurate, react 3h at 72 DEG C, add 4 parts of glycerine, react 40min at 82 DEG C,
Obtain modified polyurethane；
2nd step：By weight, catalyst is added in 70 parts of phenol, and (catalyst is sodium hydroxide and zinc oxide mole
Than for 1~1 mixture), after heating, add 7 parts of anion unsaturated monomer styrene sulfonic acid, 4 parts of urea and melamine 4
Part, it is reacted, between 45 DEG C of reaction temperature, reaction time 50min；
3rd step：In the reaction product that the 2nd step obtains, 60 parts of modified polyurethane and formaldehyde are added, is reacted, instead
Between answering 92 DEG C of temperature, reaction time 3h, after reaction, cooling discharge obtains phenol-formaldehyde resin modified；
4th step：By phenol-formaldehyde resin modified, 500 parts of water, amphoteric surfactant lauryl dimethyl oxyneurine
7 parts, 6 parts of silane coupling agent, 7 parts of silane coupling agent, antioxidant it is double（2,4- di-t-butyl -5- aminomethyl phenyls）Pentaerythrite-
Two -3 parts of phosphite esters are uniformly mixed, and obtain immersion fluid；
5th step：Block of glass wool is all infiltrated in immersion fluid for 300 parts, takes out and is placed on partition board after 30 minutes, waited for no longer
Have slurry outflow after, be placed in drying box in, at a temperature of 70 DEG C will drying to get.
Test method： GB/T 13350-2008《Class wool and their products for thermal insulation》、Q/JC JCY0029-2014《Change
Property block of glass wool》、GB/T 10295-2008《Technology of Steady State Thermal Resistance of Thermal Insulating Material and measurement heat-flow meter method in relation to characteristic》、GB
8624-2010《Construction material and product burns grading performance》、GB/T 25975-2010《External wall external thermal insulation rock wool system
Product》、GB/T 13480-1992《Mineral cotton goods compression performance test method》、JG 149-2003《Expansion joints bellows
External thermal insulation system》、GB/T 8811-2008《Rigid foam dimensional stability test method》、GB/T 10299-
2011《Test method for hydrophobic nature of thermal insulation》、GB/T 11835-2007《Thermal insulation rock wool, mineral wool and its product》.
Alkaline resistance test：The block of glass wool 1 hour of constant weight is impregnated with 10% NaOH solution, then with distillation
Water is rinsed, and is weighed after drying, and calculates the mass loss rate of block of glass wool.
As can be seen from the table, glass plate plate provided by the invention has preferable heat-insulating property and physical strength, and
Corrosion resistance is also preferable；Wherein, compared by embodiment 3 and reference examples 1 as can be seen that by the preparation in modified polyurethane
Cationic monomer is not added in the process, it is possible to reduce the thermal coefficient of block of glass wool.Being compared by embodiment 3 and reference examples 2 can
Melamine, which is added, to find out, in the 2nd step can reduce the water absorption of glass plate plate.Being compared by embodiment 3 and reference examples 3 can
To find out, lignin is added to after phenolic resin modified, the alkali corrosion resistance performance of block of glass wool can be effectively improved.
Claims (7)
1. a kind of preparation process of block of glass wool melamine modified phenolic resin, which is characterized in that include the following steps：
1st step：By weight, the polyethylene glycol for taking 10~15 parts, vacuum dehydration 2 while stirring at a temperature of 100~110 DEG C
~3h, is cooled to room temperature, be added 5~10 parts toluene di-isocyanate(TDI), 2~4 parts of cationic monomer, 2~4 parts of maleic acid, two
1~2 part of dibutyl tin laurate reacts 2~3h at 70~75 DEG C, adds 3~5 parts of glycerine, anti-at 80~85 DEG C
20~60min is answered, modified polyurethane is obtained；
2nd step：By weight, catalyst is added in 60~80 parts of phenol, after heating, adds anion unsaturated monomer
3~5 parts of 5~10 parts, 3~6 parts of lignin, 3~5 parts of urea and melamine, are reacted；
3rd step：In the reaction product that the 2nd step obtains, 50~70 parts of modified polyurethane and formaldehyde are added, is reacted, instead
After answering, cooling discharge obtains phenol-formaldehyde resin modified；
4th step：By phenol-formaldehyde resin modified, 300~600 parts of water, 5~10 parts of amphoteric surfactant, 3~7 parts of silane coupling agent,
5~10 parts of coupling agent, 2~4 parts of antioxidant are uniformly mixed, and obtain immersion fluid；
5th step：By 200~400 parts of block of glass wool, all infiltration is in immersion fluid, and 20~take out be placed on partition board after forty minutes,
After there is no slurry flow out after, be placed in drying box in, at a temperature of 30~80 DEG C will drying to get；
In 4th step, coupling agent is silane coupling agent or titanate coupling agent.
2. the preparation process of block of glass wool melamine modified phenolic resin according to claim 1, it is characterised in that：
In 1st step, cationic monomer is selected from MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, dimethylaminoethyl acrylate methyl base ammonia
Base ethyl ester or dimethyl diallyl ammonium chloride.
3. the preparation process of block of glass wool melamine modified phenolic resin according to claim 1, it is characterised in that：
In 2nd step, anion unsaturated monomer is selected from methacrylic acid, maleic acid, vinyl sulfonic acid, styrene sulfonic acid, 2-
(methyl) acrylamido -2- methyl propane sulfonic acids, 2- (methyl) acryloyl group ethane sulfonic acids and 2- (methyl) acryloyl group third
Alkyl sulfonic acid and their salt.
4. the preparation process of block of glass wool melamine modified phenolic resin according to claim 1, it is characterised in that：
In 2nd step, between 40~50 DEG C of reaction temperature, 30~60min of reaction time.
5. the preparation process of block of glass wool melamine modified phenolic resin according to claim 1, it is characterised in that：
In 2nd step, the lignin be bamboo acetic acid lignin, corncob alkali lignin, wheat stalk alkali lignin and
Any one or a few in poplar sulfate-reducing conditions.
6. the preparation process of block of glass wool melamine modified phenolic resin according to claim 1, it is characterised in that：
In 2nd step, the catalyst is the mixture of sodium hydroxide and zinc oxide, and the molar ratio of sodium hydroxide and zinc oxide is
1~1.5：1.
7. the preparation process of block of glass wool melamine modified phenolic resin according to claim 1, it is characterised in that：
In 3rd step, between 90~95 DEG C of reaction temperature, 2~4h of reaction time.
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| CN114381086A (en) * | 2020-10-22 | 2022-04-22 | 浙江欧仁新材料有限公司 | Heat and sound insulation cotton felt for large airplane |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962260A (en) * | 2005-11-10 | 2007-05-16 | 上海平板玻璃厂 | Environment-friendly formaldehyde-free glass wool |
| CN101508761A (en) * | 2009-03-13 | 2009-08-19 | 江苏文昌电子化工有限公司 | Process for preparing phenolic resin containing nitrogen |
| CN103571155A (en) * | 2012-08-08 | 2014-02-12 | 苏州维艾普新材料有限公司 | Glass cotton felt and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962260A (en) * | 2005-11-10 | 2007-05-16 | 上海平板玻璃厂 | Environment-friendly formaldehyde-free glass wool |
| CN101508761A (en) * | 2009-03-13 | 2009-08-19 | 江苏文昌电子化工有限公司 | Process for preparing phenolic resin containing nitrogen |
| CN103571155A (en) * | 2012-08-08 | 2014-02-12 | 苏州维艾普新材料有限公司 | Glass cotton felt and preparation method thereof |
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