CN108864692A - A kind of preparation method of high tenacity flame retardant polyurethane grouting material - Google Patents
A kind of preparation method of high tenacity flame retardant polyurethane grouting material Download PDFInfo
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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
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
- C08L75/08—Polyurethanes from polyethers
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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
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3215—Polyhydroxy compounds containing aromatic groups or benzoquinone groups
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- 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
- C08G18/50—Polyethers having heteroatoms other than oxygen
- C08G18/5021—Polyethers having heteroatoms other than oxygen having nitrogen
- C08G18/5051—Polyethers having heteroatoms other than oxygen having nitrogen containing cyano groups
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- 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
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- 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
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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Abstract
The present invention relates to a kind of preparation methods of high tenacity flame retardant polyurethane grouting material, belong to construction material preparation technical field.Bamboo chip is placed in boiling in urea and ammonia water mixture first by the present invention, the bamboo chip after boiling is placed in boiling in sodium hydroxide solution again, extract bamboo fibre, rancid reaction in greenhouse, which is put into, with castor oil immersion again obtains solidliquid mixture, ammonium polyphosphate is put into heating in water bath for reaction in melamine solution again, the product dried after reaction again reacts to obtain modified ammonium polyphosphate with monoalkoxytitanates, finally by polyphenyl polymethylene polyisocyanates, 4, 4 '-methyl diphenylene diisocyanates and hydroquinone reaction polyurethane slurry material and it is rancid after solidliquid mixture and modified ammonium polyphosphate high tenacity flame retardant polyurethane grouting material is mixed to obtain, the grouting material toughness is strong, good flame resistance, it has broad application prospects.
Description
Technical field
The present invention relates to construction material preparation technical fields, and in particular to a kind of high tenacity flame retardant polyurethane grouting material
Preparation method.
Background technique
With the rapid development of our country's economy, energy shortages promotes coal mining industry to greatly develop, and a batch is large-scale, high yield is high
The well industrial and mineral of effect is gone into operation one after another, and traditional Coal Exploitation increases deeply, but also brings a series of problems therewith.Many underground engineerings,
In the long-term use process, concrete is because easily leading to defect, slowly cracking, drop mechanical property significantly by various stress
It is low, great loss is caused to national economy.
Grouting technique by composition slurry material different demarcation be：Cement grout, cement mortar grouting, clay grouting, water
Mud clay grouting, cement-sodium silicate grouting and Polymer Solution chemical grouting.So far, cement is still and answers in grouting works
With widest basic material.But because cement grouting material metal particles profile material, cannot obtain the processing of certain micro-cracks
Satisfied effect.Chemical grouting material have viscosity is low, concrete castability is good, penetration is strong, filling is closely knit, good waterproof performance and starch material
The advantages that intensity is high after consolidation.Therefore, to the unsatisfactory grouting works of cement grouting material, multiselect chemical grouting material.
With regard to for for handling the chemical grouting material of distress in concrete, polyurethane grouting material to be because of its superior performance, in water conservancy, water
It is widely used in the engineerings such as electricity, tunnel, subway, mine, industrial building.
Polyurethane grouting material is that polyurethane resin is applied to play reinforcing, water blockoff, antiseepage in civil construction project
A kind of new material.Hydrophobic polyurethane grouting material reacted with water the foams to be formed be fragile material, if building structure because
It settles or expands with heat and contract with cold and deformation occur, then easily lead to material cracks and multiple leakage occurs, the durability of impervious leakage-stopping is lower.It is existing
Polyurethane grouting material be not suitable for the elastic packing in the crack at the dry position of building structure, seam and hole.In addition, by
Such as acetone, dimethylbenzene low-flash flammable solvent are added in existing polyurethane grouting material, wherein the flash-point of acetone
It is -17.8 DEG C, the flash-point of dimethylbenzene is 27.2~46.1 DEG C, therefore very high to the fire protection requirement of construction site, careless slightly
Major accident will be led to.Furthermore since these solvents, plasticizer itself have stronger volatility and toxicity, is producing and making
With adverse effect is brought to environmental protection and human health in the process, it could even be possible to generating serious consequence.
Therefore, developing a kind of polyurethane grouting material for being able to solve above-mentioned performance issue is highly desirable.
Summary of the invention
The technical problems to be solved by the invention：The bubble to be formed is reacted with water for polyurethane grouting material common at present
Foam body is fragile material, is easy to cause material cracks and multiple leakage occurs, and durability and the fire protecting performance difference of impervious leakage-stopping lack
It falls into, provides a kind of preparation method of high tenacity flame retardant polyurethane grouting material.
In order to solve the above technical problems, the technical solution adopted by the present invention is that：
A kind of preparation method of high tenacity flame retardant polyurethane grouting material, it is characterised in that specifically preparation step is：
（1）It is in mass ratio 2:1 will urea liquid and ammonium hydroxide mix after contain in beaker, obtain mixed liquor, then by mixed liquor and
Bamboo chip is put into beaker, and beaker is put into water-bath and heats boiling, takes out bamboo chip, washing；
（2）By after above-mentioned washing bamboo chip and sodium hydroxide solution mix be placed in beaker, place the beaker in water-bath, add
Heat is warming up to 80~85 DEG C of 1.0~1.5h of boiling, is continuously heating to 90~95 DEG C of 1.5~2.0h of boiling, takes out after the completion of heating
Bamboo chip is rinsed with clear water, is put into mortar, is tapped to bamboo fibre with stone pestle into silk, is put in Indoor Natural and dries, after drying
It pours into stainless steel pallet after bamboo silk and castor oil mixing, impregnates indoors, then stainless steel pallet is put into rancid anti-in greenhouse
It answers, obtains rancid product, it is spare；
（3）15~20g ammonium polyphosphate is taken to be put into the beaker for the melamine solution that 200mL mass fraction is 20~30%, then will
Beaker, which is put into water-bath, to react, and after reaction, is put into baking oven, drying obtains solid；
（4）The above-mentioned solid of 15~20g is put into the beaker for filling 200mL monoalkoxytitanates, beaker is put into water-bath
Middle reaction is put into baking oven and dries to obtain modified solid after reaction, then modified solid is put into grinder and grinds to produce
Object, it is spare；
（5）By polyphenyl polymethylene polyisocyanates, 4,4 '-methyl diphenylene diisocyanates, hydroquinone investment reaction
In kettle, it is stirred to obtain mixed liquor, takes paracyanogen propylene glycol to be put into dehydration device and is dehydrated, is gradually added dropwise into mixed liquor mixed
The dewatered paracyanogen propylene glycol of the quality such as liquid is closed, keeping dropping temperature is 20~30 DEG C, and is controlled under nitrogen protection
Drop rate drips off in 1.0~1.5h；
（6）After above-mentioned be added dropwise to complete, reaction kettle is heated up, isothermal reaction obtains reaction solution, extracts reaction solution, spare rancid production
Object, ammonium hypophosphite, spare product are put into stirring in blender and discharge to get the fire-retardant hydrophobic polyurethane injection material of high tenacity
Material.
Step（1）Described in the mass fraction of urea liquid be 30%, the mass fraction of ammonium hydroxide is 30%, the quality of bamboo chip
Mixed liquor quality 5% is accounted for, heating water bath boiling temperature is 100 DEG C, and digestion time is 1.5~1.8h.
Step（2）Described in bamboo chip and sodium hydroxide solution mass ratio be 1:10, the quality point of sodium hydroxide solution
Number is 1~3%, and the mass ratio of bamboo silk and castor oil after drying is 1:5, indoor soaking time is 36~38h, the air in greenhouse
Relative humidity is 60~70%, temperature is 35~42 DEG C, and standing time is 3~5 days.
Step（3）Described in water bath temperature be 50~60 DEG C, being put in water-bath the reaction time is 2~3h, baking oven
Temperature is 105~110 DEG C.
Step（4）Described in the temperature of water-bath be 70~80 DEG C, the reaction time is 1.5~2.0h, and oven temperature is
105~110 DEG C, the milling time of grinder is 0.4~0.6h.
Step（5）Described in polyphenyl polymethylene polyisocyanates, 4,4 '-methyl diphenylene diisocyanates, right
Benzenediol according to parts by weight, respectively 50~60 parts, 50~60 parts and 25~30 parts, be dehydrated environment pressure be 0.5~
0.6kPa, temperature are 110~120 DEG C, 2~3h of dewatering time.
Step（6）Described in reaction kettle warming temperature to 55~60 DEG C, the isothermal reaction time is 2.0~2.5h, reaction
Liquid, rancid product, ammonium hypophosphite, spare product according to parts by weight, respectively 80~100 parts, 20~30 parts, 8~10 parts,
8~10 parts, the stirring rate of blender is 80~100r/min, and mixing time is 0.5~1.0h.
The method have the benefit that：
Bamboo chip is placed in boiling in urea and ammonia water mixture first by the present invention, then that the bamboo chip after boiling is placed in sodium hydroxide is molten
Bamboo fibre is extracted in boiling in liquid, is put into rancid reaction in greenhouse with castor oil immersion and obtains rancid product, then ammonium polyphosphate is put
Enter heating in water bath for reaction in melamine solution, the product and monoalkoxytitanates to which after reaction, drying is obtained are anti-
Modified ammonium polyphosphate should be obtained, finally by polyphenyl polymethylene polyisocyanates, 4,4 '-diphenylmethane diisocyanates
Polyurethane slurry material that ester and hydroquinone react and it is rancid after solidliquid mixture and modified ammonium polyphosphate it is mixed
Conjunction stirs to get high tenacity flame retardant polyurethane grouting material, and using the bamboo fibre of high tenacity as raw material, bamboo fibre itself is the present invention
A kind of natural reproducible material, there is very high specific strength, and in natural fiber, the intensity highest of bamboo fibre has good resistance to
Fatigability and fail-safety, bamboo fibre are impregnated by castor oil, then by corrode it is rancid after, using rancid microorganism by castor-oil plant
Oil degradation, generates a large amount of hydrophobicity ester groups and alkyl, then obtained ester group and alkyl are introduced into bamboo fibre in process of spoilage
Dimension table face enables bamboo fibre surface to reduce, and is dissolved in oiliness grouting material matrix, adds to more facilitate bamboo fibre
Bamboo fibre oiliness adsorption capacity with higher itself, is more soluble in bamboo fibre in grouting material, and the addition of bamboo fibre is to grouting
Stress conducting path is introduced in material, to enhance the tensile strength of grouting material, grouting material is made to have more toughness；
（2）Modified ammonium polyphosphate is added in grouting material the present invention, and ammonium polyphosphate is cyanurotriamide modified first, utilizes
Melamine coated ammonium polyphosphate, when burning, decomposes to give off so that the flame retardant property of ammonium polyphosphate is more prominent
Ammonia generates the films such as volatility phosphorous oxides or polyphosphoric acid and air exclusion simultaneously, achievees the effect that isolation is fire-retardant, then will
Ammonium polyphosphate is modified with coupling agent, and coupling agent itself has anti-flammability, and is to have organophilic group, can be passed through
Hydrogen bond is generated with polymer to be more soluble in wherein, not only effectively enhances the anti-flammability of grouting material, moreover it is possible to improve grouting material
Toughness and heat resistance, have broad application prospects.
Specific embodiment
It is in mass ratio 2:1 by mass fraction be 30% urea liquid and mass fraction be 30% ammonium hydroxide mix be placed on
In beaker 1, mixed liquor is obtained, the bamboo chip of mixed liquor quality 5% is put into beaker 1, then beaker 1 is placed in 100 DEG C of water-baths and is added
Hot 1.5~1.8h of boiling takes out bamboo chip, washing；It is in mass ratio 1:10 by after above-mentioned washing bamboo chip and mass fraction be 1~
The mixing of 3% sodium hydroxide solution is placed in beaker 2, and beaker 2 is placed in water-bath, is heated to 80~85 DEG C, boiling
1.0~1.5h is continuously heating to 90~95 DEG C, 1.5~2.0h of boiling, takes out bamboo chip after the completion of heating and rinsed with clear water, is put into
It in mortar, is tapped to bamboo fibre with stone pestle into silk, is put in Indoor Natural and dries, the bamboo silk and castor oil after drying are in mass ratio
It is 1:It is poured into stainless steel pallet after 5 mixing, impregnates 36~38h indoors, then stainless steel pallet is put into relative air humidity
Rancid reaction 3~5 days, obtain rancid product in the greenhouse for being 35~42 DEG C for 60~70%, temperature, spare；Take 15~20g poly-
Ammonium phosphate is put into the beaker 3 for filling the melamine solution that 200mL mass fraction is 20~30%, then beaker 3 is put into 50~
In 60 DEG C of water-bath, 2~3h is reacted, to after reaction, be put into baking oven, dries, obtains at being 105~110 DEG C in temperature
To solid；The above-mentioned solid of 10~15g is put into the beaker 4 for filling 200mL monoalkoxytitanates, beaker 4 is put into 70~
In 80 DEG C of water-bath, 1.5~2.0h is reacted, to after reaction, be put into baking oven, is dried at being 105~110 DEG C in temperature
Modified solid is obtained, then modified solid is put into 0.4~0.6h of grinding in grinder, obtains grinding product, it is spare；By weight
Number meter, by 50~60 parts of polyphenyl polymethylene polyisocyanates, 50~60 part 4,4 '-methyl diphenylene diisocyanates, 25
In~30 parts of hydroquinone investment reaction kettles, it is stirred to obtain mixed liquor, paracyanogen propylene glycol is put into dehydration device,
It is dehydrated 2~3h in the environment of pressure is 0.5~0.6kPa, temperature is 110~120 DEG C, mixing is gradually added dropwise into mixed liquor
The dewatered paracyanogen propylene glycol of the quality such as liquid, keeping dropping temperature is 20~30 DEG C, and control drop under nitrogen protection
Rate of acceleration drips off in 1.0~1.5h；After above-mentioned be added dropwise to complete, reaction kettle is warming up to 55~60 DEG C, isothermal reaction 2.0
~2.5h obtains reaction solution, according to parts by weight, takes 80~100 parts of reaction solutions, 20~30 parts of spare rancid products, 8~10
Part ammonium hypophosphite, 8~10 parts of spare grinding products, which are put into blender, stirs 0.5~1.0h with the revolving speed of 80~100r/min
After discharge to get the fire-retardant hydrophobic polyurethane grouting material of high tenacity.
It is in mass ratio 2:1 by mass fraction be 30% urea liquid and mass fraction be 30% ammonium hydroxide mix be placed on
In beaker 1, mixed liquor is obtained, the bamboo chip of mixed liquor quality 5% is put into beaker 1, then beaker 1 is placed in 100 DEG C of water-baths and is added
Hot boiling 1.5h takes out bamboo chip, washing；It is in mass ratio 1:10 by after above-mentioned washing bamboo chip and mass fraction be 1% hydroxide
Sodium solution mixing is placed in beaker 2, and beaker 2 is placed in water-bath, is heated to 80 DEG C, boiling 1.0h continues to heat up
To 90 DEG C, boiling 1.5h, heating after the completion of take out bamboo chip rinsed with clear water, be put into mortar, with stone pestle tap to bamboo fibre at
Silk, is put in Indoor Natural and dries, and the bamboo silk and castor oil after drying are 1 in mass ratio:Stainless steel pallet is poured into after 5 mixing
In, impregnate 36h indoors, then stainless steel pallet is put into rancid anti-in the greenhouse that relative air humidity is 60%, temperature is 35 DEG C
It answers 3 days, obtains rancid product, it is spare；It takes 15g ammonium polyphosphate to be put into and fills the melamine solution that 200mL mass fraction is 20%
Beaker 3 in, then beaker 3 is put into 50 DEG C of water-bath, react 2h to after reaction, be put into baking oven is in temperature
It is dried at 105 DEG C, obtains solid；The above-mentioned solid of 10g is put into the beaker 4 for filling 200mL monoalkoxytitanates, by beaker
4 are put into 70 DEG C of water-bath, react 1.5h, to after reaction, be put into baking oven, dry and obtain at being 105 DEG C in temperature
Modified solid, then modified solid is put into grinder and grinds 0.4h, grinding product is obtained, it is spare；According to parts by weight, by 50
Part polyphenyl polymethylene polyisocyanates, 50 part 4,4 '-methyl diphenylene diisocyanates, 25 parts of hydroquinones investment reactions
It in kettle, is stirred to obtain mixed liquor, paracyanogen propylene glycol is put into dehydration device, pressure is 0.5kPa, temperature is
It is dehydrated 2h in the environment of 110 DEG C, the dewatered paracyanogen propylene glycol of the quality such as mixed liquor is gradually added dropwise into mixed liquor, protects
Holding dropping temperature is 20 DEG C, and controls drop rate under nitrogen protection, is dripped off in 1.0h；It, will after above-mentioned be added dropwise to complete
Reaction kettle is warming up to 55 DEG C, and isothermal reaction 2.0h obtains reaction solution, according to parts by weight, take 80 parts of reaction solutions, 20 parts it is spare
Rancid product, 8 parts of ammonium hypophosphites, 8 parts of spare grinding products are put into blender to go out after the revolving speed stirring 0.5h of 80r/min
Material is to get the fire-retardant hydrophobic polyurethane grouting material of high tenacity.
It is in mass ratio 2:1 by mass fraction be 30% urea liquid and mass fraction be 30% ammonium hydroxide mix be placed on
In beaker 1, mixed liquor is obtained, the bamboo chip of mixed liquor quality 5% is put into beaker 1, then beaker 1 is placed in 100 DEG C of water-baths and is added
Hot boiling 1.7h takes out bamboo chip, washing；It is in mass ratio 1:10 by after above-mentioned washing bamboo chip and mass fraction be 2% hydroxide
Sodium solution mixing is placed in beaker 2, and beaker 2 is placed in water-bath, is heated to 83 DEG C, boiling 1.4h continues to heat up
To 93 DEG C, boiling 1.7h, heating after the completion of take out bamboo chip rinsed with clear water, be put into mortar, with stone pestle tap to bamboo fibre at
Silk, is put in Indoor Natural and dries, and the bamboo silk and castor oil after drying are 1 in mass ratio:Stainless steel pallet is poured into after 5 mixing
In, impregnate 37h indoors, then stainless steel pallet is put into rancid anti-in the greenhouse that relative air humidity is 65%, temperature is 38 DEG C
It answers 4 days, obtains rancid product, it is spare；It takes 18g ammonium polyphosphate to be put into and fills the melamine solution that 200mL mass fraction is 25%
Beaker 3 in, then beaker 3 is put into 55 DEG C of water-bath, react 2h to after reaction, be put into baking oven is in temperature
It is dried at 17 DEG C, obtains solid；The above-mentioned solid of 13g is put into the beaker 4 for filling 200mL monoalkoxytitanates, by beaker 4
It is put into 75 DEG C of water-bath, reacts 1.7h, to after reaction, be put into baking oven, dry and changed at being 107 DEG C in temperature
Property solid, then modified solid is put into grinder and grinds 0.5h, grinding product is obtained, it is spare；According to parts by weight, by 55 parts
Polyphenyl polymethylene polyisocyanates, 55 part 4,4 '-methyl diphenylene diisocyanates, 27 parts of hydroquinones put into reaction kettle
In, be stirred to obtain mixed liquor, paracyanogen propylene glycol be put into dehydration device, pressure be 0.5kPa, temperature 115
It is dehydrated 2.5h in the environment of DEG C, the dewatered paracyanogen propylene glycol of the quality such as mixed liquor is gradually added dropwise into mixed liquor, protects
Holding dropping temperature is 25 DEG C, and controls drop rate under nitrogen protection, is dripped off in 1.3h；It, will after above-mentioned be added dropwise to complete
Reaction kettle is warming up to 57 DEG C, and isothermal reaction 2.3h obtains reaction solution, according to parts by weight, take 90 parts of reaction solutions, 25 parts it is spare
Rancid product, 9 parts of ammonium hypophosphites, 9 parts of spare grinding products are put into blender to go out after the revolving speed stirring 0.7h of 85r/min
Material is to get the fire-retardant hydrophobic polyurethane grouting material of high tenacity.
It is in mass ratio 2:1 by mass fraction be 30% urea liquid and mass fraction be 30% ammonium hydroxide mix be placed on
In beaker 1, mixed liquor is obtained, the bamboo chip of mixed liquor quality 5% is put into beaker 1, then beaker 1 is placed in 100 DEG C of water-baths and is added
Hot boiling 1.8h takes out bamboo chip, washing；It is in mass ratio 1:10 by after above-mentioned washing bamboo chip and mass fraction be 3% hydroxide
Sodium solution mixing is placed in beaker 2, and beaker 2 is placed in water-bath, is heated to 85 DEG C, boiling 1.5h continues to heat up
To 95 DEG C, boiling 2.0h, heating after the completion of take out bamboo chip rinsed with clear water, be put into mortar, with stone pestle tap to bamboo fibre at
Silk, is put in Indoor Natural and dries, and the bamboo silk and castor oil after drying are 1 in mass ratio:Stainless steel pallet is poured into after 5 mixing
In, impregnate 38h indoors, then stainless steel pallet is put into rancid anti-in the greenhouse that relative air humidity is 70%, temperature is 42 DEG C
It answers 5 days, obtains rancid product, it is spare；It takes 20g ammonium polyphosphate to be put into and fills the melamine solution that 200mL mass fraction is 30%
Beaker 3 in, then beaker 3 is put into 60 DEG C of water-bath, react 3h to after reaction, be put into baking oven is in temperature
It is dried at 110 DEG C, obtains solid；The above-mentioned solid of 15g is put into the beaker 4 for filling 200mL monoalkoxytitanates, by beaker
4 are put into 80 DEG C of water-bath, react 2.0h, to after reaction, be put into baking oven, dry and obtain at being 110 DEG C in temperature
Modified solid, then modified solid is put into grinder and grinds 0.6h, grinding product is obtained, it is spare；According to parts by weight, by 60
Part polyphenyl polymethylene polyisocyanates, 60 part 4,4 '-methyl diphenylene diisocyanates, 30 parts of hydroquinones investment reactions
It in kettle, is stirred to obtain mixed liquor, paracyanogen propylene glycol is put into dehydration device, pressure is 0.6kPa, temperature is
It is dehydrated 3h in the environment of 120 DEG C, the dewatered paracyanogen propylene glycol of the quality such as mixed liquor is gradually added dropwise into mixed liquor, protects
Holding dropping temperature is 30 DEG C, and controls drop rate under nitrogen protection, is dripped off in 1.5h；It, will after above-mentioned be added dropwise to complete
Reaction kettle is warming up to 60 DEG C, and isothermal reaction 2.5h obtains reaction solution, according to parts by weight, take 100 parts of reaction solutions, 30 parts it is spare
Rancid product, 10 parts of ammonium hypophosphites, 10 parts of spare grinding products are put into blender and are stirred with the revolving speed of 100r/min
Discharging is after 1.0h to get the fire-retardant hydrophobic polyurethane grouting material of high tenacity.
The grouting material that comparative example is produced with company of Beijing is as a comparison case
Grouting material in high tenacity flame retardant polyurethane grouting material produced by the present invention and comparative example is detected, detection knot
Fruit is as shown in table 1：
By example 1~3 prepared by the present invention and comparative example, it is made having a size of 100mm × 100mm × 500mm test specimen, pours
After test specimen is moved in standard curing room conserve rapidly, tested when maintenance was to 28 days.
Intensity test
It is measured referring to GB/T2567-2008 standard.
1 performance measurement result of table
From the data in table 1, it can be seen that high tenacity flame retardant polyurethane grouting material produced by the present invention, good mechanical properties, toughness is strong,
Deformation is not susceptible in varying environment, and anti-flammability is strong, antiseep effect is good, has wide prospect of the application.
Claims (7)
1. a kind of preparation method of high tenacity flame retardant polyurethane grouting material, it is characterised in that specifically preparation step is：
（1）It is in mass ratio 2:1 will urea liquid and ammonium hydroxide mix after contain in beaker, obtain mixed liquor, then by mixed liquor and
Bamboo chip is put into beaker, and beaker is put into water-bath and heats boiling, takes out bamboo chip, washing；
（2）By after above-mentioned washing bamboo chip and sodium hydroxide solution mix be placed in beaker, place the beaker in water-bath, add
Heat is warming up to 80~85 DEG C of 1.0~1.5h of boiling, is continuously heating to 90~95 DEG C of 1.5~2.0h of boiling, takes out after the completion of heating
Bamboo chip is rinsed with clear water, is put into mortar, is tapped to bamboo fibre with stone pestle into silk, is put in Indoor Natural and dries, after drying
It pours into stainless steel pallet after bamboo silk and castor oil mixing, impregnates indoors, then stainless steel pallet is put into rancid anti-in greenhouse
It answers, obtains rancid product, it is spare；
（3）15~20g ammonium polyphosphate is taken to be put into the beaker for the melamine solution that 200mL mass fraction is 20~30%, then will
Beaker, which is put into water-bath, to react, and after reaction, is put into baking oven, drying obtains solid；
（4）The above-mentioned solid of 15~20g is put into the beaker for filling 200mL monoalkoxytitanates, beaker is put into water-bath
Middle reaction is put into baking oven and dries to obtain modified solid after reaction, then modified solid is put into grinder and grinds to produce
Object, it is spare；
（5）By polyphenyl polymethylene polyisocyanates, 4,4 '-methyl diphenylene diisocyanates, hydroquinone investment reaction
In kettle, it is stirred to obtain mixed liquor, takes paracyanogen propylene glycol to be put into dehydration device and is dehydrated, is gradually added dropwise into mixed liquor mixed
The dewatered paracyanogen propylene glycol of the quality such as liquid is closed, keeping dropping temperature is 20~30 DEG C, and is controlled under nitrogen protection
Drop rate drips off in 1.0~1.5h；
（6）After above-mentioned be added dropwise to complete, reaction kettle is heated up, isothermal reaction obtains reaction solution, extracts reaction solution, spare rancid production
Object, ammonium hypophosphite, spare product are put into stirring in blender and discharge to get the fire-retardant hydrophobic polyurethane injection material of high tenacity
Material.
2. a kind of preparation method of high tenacity flame retardant polyurethane grouting material according to claim 1, it is characterised in that：Step
Suddenly（1）Described in the mass fraction of urea liquid be 30%, the mass fraction of ammonium hydroxide is 30%, and the quality of bamboo chip accounts for mixed liquor matter
Amount 5%, heating water bath boiling temperature are 100 DEG C, and digestion time is 1.5~1.8h.
3. a kind of preparation method of high tenacity flame retardant polyurethane grouting material according to claim 1, it is characterised in that：Step
Suddenly（2）Described in bamboo chip and sodium hydroxide solution mass ratio be 1:10, the mass fraction of sodium hydroxide solution is 1~3%,
The mass ratio of bamboo silk and castor oil after drying is 1:5, indoor soaking time is 36~38h, and the relative air humidity in greenhouse is
60~70%, temperature is 35~42 DEG C, and standing time is 3~5 days.
4. a kind of preparation method of high tenacity flame retardant polyurethane grouting material according to claim 1, it is characterised in that：Step
Suddenly（3）Described in water bath temperature be 50~60 DEG C, being put in water-bath the reaction time is 2~3h, oven temperature is 105~
110℃。
5. a kind of preparation method of high tenacity flame retardant polyurethane grouting material according to claim 1, it is characterised in that：Step
Suddenly（4）Described in water-bath temperature be 70~80 DEG C, the reaction time be 1.5~2.0h, oven temperature be 105~110 DEG C,
The milling time of grinder is 0.4~0.6h.
6. a kind of preparation method of high tenacity flame retardant polyurethane grouting material according to claim 1, it is characterised in that：Step
Suddenly（5）Described in polyphenyl polymethylene polyisocyanates, 4,4 '-methyl diphenylene diisocyanates, hydroquinone by weight
Number meter is measured, respectively 50~60 parts, 50~60 parts and 25~30 parts, the pressure for being dehydrated environment is 0.5~0.6kPa, and temperature is
110~120 DEG C, 2~3h of dewatering time.
7. a kind of preparation method of high tenacity flame retardant polyurethane grouting material according to claim 1, it is characterised in that：Step
Suddenly（6）Described in reaction kettle warming temperature to 55~60 DEG C, the isothermal reaction time is 2.0~2.5h, reaction solution, rancid production
Object, ammonium hypophosphite, spare product according to parts by weight, respectively 80~100 parts, 20~30 parts, 8~10 parts, 8~10 parts,
The stirring rate of blender is 80~100r/min, and mixing time is 0.5~1.0h.
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