CN108192330A - A kind of preparation method of toughening leakproof polyurethane grouting material - Google Patents
A kind of preparation method of toughening leakproof polyurethane grouting material Download PDFInfo
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- CN108192330A CN108192330A CN201711254831.1A CN201711254831A CN108192330A CN 108192330 A CN108192330 A CN 108192330A CN 201711254831 A CN201711254831 A CN 201711254831A CN 108192330 A CN108192330 A CN 108192330A
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- parts
- grouting material
- polyurethane
- leakproof
- toughening
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- 229920002635 polyurethane Polymers 0.000 title claims abstract description 68
- 239000004814 polyurethane Substances 0.000 title claims abstract description 68
- 239000000463 material Substances 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002002 slurry Substances 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 239000000835 fiber Substances 0.000 claims abstract description 21
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 20
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims abstract description 14
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims abstract description 14
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000010451 perlite Substances 0.000 claims abstract description 13
- 235000019362 perlite Nutrition 0.000 claims abstract description 13
- 235000011187 glycerol Nutrition 0.000 claims abstract description 10
- 229920001131 Pulp (paper) Polymers 0.000 claims description 37
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000002023 wood Substances 0.000 claims description 17
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 16
- 238000004821 distillation Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 229920002522 Wood fibre Polymers 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 239000000047 product Substances 0.000 claims description 11
- 238000013019 agitation Methods 0.000 claims description 8
- 238000003763 carbonization Methods 0.000 claims description 8
- 238000010790 dilution Methods 0.000 claims description 8
- 239000012895 dilution Substances 0.000 claims description 8
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000005360 mashing Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical class CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical class O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- 235000019260 propionic acid Nutrition 0.000 claims description 6
- 239000002893 slag Substances 0.000 claims description 6
- 150000004672 propanoic acids Chemical class 0.000 claims description 5
- 150000008065 acid anhydrides Chemical class 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000010009 beating Methods 0.000 claims description 2
- 239000006227 byproduct Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims 1
- 230000005494 condensation Effects 0.000 claims 1
- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical compound C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 claims 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000002708 enhancing effect Effects 0.000 abstract description 2
- 239000012948 isocyanate Substances 0.000 abstract description 2
- 230000008719 thickening Effects 0.000 abstract description 2
- DBXBTMSZEOQQDU-UHFFFAOYSA-N 3-hydroxyisobutyric acid Chemical compound OCC(C)C(O)=O DBXBTMSZEOQQDU-UHFFFAOYSA-N 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 4
- 239000004568 cement Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- 239000004567 concrete Substances 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical class OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 2
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 2
- 235000011613 Pinus brutia Nutrition 0.000 description 2
- 241000018646 Pinus brutia Species 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002304 perfume Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 235000013599 spices Nutrition 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 239000011083 cement mortar Substances 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000009429 distress Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 239000011440 grout Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910001562 pearlite Inorganic materials 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- 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
-
- 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
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
-
- 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
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4081—Mixtures of compounds of group C08G18/64 with other macromolecular compounds
-
- 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
- C08G18/4825—Polyethers containing two hydroxy groups
-
- 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
- C08G18/64—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63
-
- 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
- C08G18/6692—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/34
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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
- C08G18/73—Polyisocyanates or polyisothiocyanates acyclic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09F—NATURAL RESINS; FRENCH POLISH; DRYING-OILS; OIL DRYING AGENTS, i.e. SICCATIVES; TURPENTINE
- C09F1/00—Obtaining purification, or chemical modification of natural resins, e.g. oleo-resins
- C09F1/04—Chemical modification, e.g. esterification
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- C—CHEMISTRY; METALLURGY
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Polyurethanes Or Polyureas (AREA)
- Soil Conditioners And Soil-Stabilizing Materials (AREA)
Abstract
The present invention relates to grouting material preparing technical fields, and in particular to a kind of preparation method of toughening leakproof polyurethane grouting material.The present invention makes by oneself to obtain carbonized woody fiber using fir timber as raw material, perlite with vitrifying microballon by certain mass ratio is mixed to get and mixes aggregate, polyetherdiol and rosin are dispersed with stirring, add di-isocyanate, hydroxymethyl propionic acid, glycerine, the raw materials such as maleic anhydride, polyurethane slurry is obtained by the reaction, homemade carbonized wooden fiber is mixed into polyurethane slurry, mix aggregate, by toughening leakproof polyurethane grouting material is obtained by the reaction, carbonized wooden fiber has strong thickening enhancing effect, so as to improve the toughness of polyurethane grouting material, it mixes in aggregate containing expanded perlite and vitrifying microballon, so as to which polyurethane grouting material be made to be influenced to become smaller by expanding with heat and contract with cold, possess preferable impervious leakage-stopping function, it has a extensive future.
Description
Technical field
The present invention relates to grouting material preparing technical fields, and in particular to a kind of system of toughening leakproof polyurethane grouting material
Preparation Method.
Background technology
With the fast development of China'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,
During long-term use, concrete is because by various stress, easily leading to defect, slowly cracking, mechanical property is made significantly to drop
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 is answered in grouting works
With widest basic material.But because cement grouting material metal particles section bar 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, the unsatisfactory grouting works to cement grouting material, multiselect chemical grouting material.
For for handling the chemical grouting material of distress in concrete, polyurethane grouting material is 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.Polyurethane grouting material includes hydrophilic polyurethane grouting material and hydrophobic polyurethane grouting material.Often
The waterborne polyurethane grouting material of rule has good hydrophilic property, meets water and reacts rapidly, induration of the generation with certain elasticity, packet
Water is big, the features such as up to 15~20 times, plays the effect of quick water blockoff well.But waterborne polyurethane grouting material
Material must use under long-term moist environment, and otherwise easy drying shrinkage after dehydration, causes to reappear leakage, not be suitable for dry or dry
In environment under wet cycling condition.Hydrophobic polyurethane grouting material reacts the foams to be formed with water for fragile material, if building
There is deformation because settling or expanding with heat and contract with cold in building structure, then easily leads to material cracks and multiple leakage occurs, the durability of impervious leakage-stopping
It is relatively low.The elasticity that existing polyurethane grouting material is not suitable for the building structure drying crack at position, seam and hole is close
Envelope.In addition, due to being added to such as acetone, dimethylbenzene low-flash flammable solvent in existing polyurethane grouting material, wherein, third
The flash-point of ketone is -17.8 DEG C, and the flash-point of dimethylbenzene is 27.2~46.1 DEG C, therefore very high to the fire protection requirement of construction site,
It is careless slightly to lead to major accident.Furthermore since these solvents, plasticizer have stronger volatility and toxicity in itself,
Adverse effect is brought to environmental protection and health during production and use, it could even be possible to generating serious consequence.
Therefore, developing a kind of polyurethane grouting material that can solve above-mentioned performance issue is highly desirable.
Invention content
Present invention mainly solves the technical issues of, react with water tough after generation microcellular structure for polyurethane grouting material
Property it is poor and easily generate deformation because expanding with heat and contract with cold, the defects of so as to leak, provide a kind of toughening leakproof polyurethane
The preparation method of grouting material.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of toughening leakproof polyurethane grouting material, it is characterised in that specifically preparation process is：
（1）Fir timber is placed in pulverizer and is crushed, obtains sawdust, 400~450g sawdusts are placed in mill, into mill
600~700mL water is added in, grinding mashing obtains wood pulp, 40~50g phenol, 20~25g hexa-methylenes four are added in into wood pulp
Amine is stirred under room temperature, is stood, is obtained Wood liquefied wood pulp；
（2）200~300mL acetone is added in into Wood liquefied wood pulp, is filtered after agitation and dilution, removes wooden slag, obtains purifying wood
Slurry, purifying wood pulp is placed in the cucurbit with condensing unit, heat temperature raising, and distillation obtains product of distillation, by product of distillation
It is placed in baking oven, heat temperature raising, it is dry, obtain wood fibre；
（3）Wood fibre is placed in calcining furnace, stove evacuation, heat temperature raising will be calcined, high temperature carbonization obtains carbonized wooden fibre
Dimension, expanded perlite is mixed with vitrifying microballon, obtains mixing aggregate；
（4）Count in parts by weight, into the dry three-necked flask with condensing unit add in 30~40 parts of polyetherdiol, 20~
30 parts of rosin, under nitrogen protection, temperature programming, and disperseed with magnetic stirrer；
（5）It counts in parts by weight, 80~90 parts of hexamethylene diisocyanates is added in into above-mentioned three-necked flask, the reaction was continued, treats three mouthfuls
Flask cools down, and adds in 10~15 parts of dihydromethyl propionic acids, 20~30 parts of glycerine and 20~25 parts of Malaysias into three-necked flask successively
Acid anhydrides after 3~5 parts of dibutyl tin laurates are dissolved in 35~40 parts of acetone, is instilled with constant pressure funnel in three-necked flask,
It heats up when being added dropwise, the reaction was continued, obtains polyurethane slurry；
（6）Count in parts by weight, added in into 70~80 parts of polyurethane slurries 12~15 parts of carbonized wooden fibers, 30~40 parts it is mixed
Aggregate is closed, under stirring, continues to add in 0.8~1.0 part of triethylamine into polyurethane slurry, stirring is improved after reaction and is turned
Speed is dispersed with stirring, and obtains toughening leakproof polyurethane grouting material.
Step（1）The grinding time be 30~45min, grinding beating time be 3~4h, mixing time be 30~
40min, time of repose are 4~5h.
Step（2）The agitation and dilution time is 3~5min, and temperature is 100~110 DEG C after heat temperature raising, during distillation
Between for 4~6h, temperature is 90~100 DEG C after heat temperature raising, and drying time is 4~5h.
Step（3）After the heat temperature raising temperature be 600~650 DEG C, the high temperature carbonization time be 3~4h, expanded pearlite
The grain size of rock is 200 mesh, and the grain size of vitrifying microballon is 0.1~0.2mm, the quality that expanded perlite is mixed with vitrifying microballon
Than for 1 ︰ 3.
Step（4）The heating rate is 3~5 DEG C/min, and temperature is 90~100 DEG C after heating, and magnetic stirring apparatus turns
Speed is 200~300r/min, is dispersed with stirring the time as 30~40min.
Step（5）The reaction was continued time is 2~3h, and temperature is 50~60 DEG C after three-necked flask cooling, and speed is added dropwise
Rate is 2~3mL/min, and control heating rate is 3~5 DEG C/min, and temperature is 80~82 DEG C after heating, and the reaction was continued, and the time is 3
~4h.
Step（6）The speed of agitator is 300~400r/min, and the reaction time is 5~7min, after improving speed of agitator
Rotating speed is 600~800r/min, is dispersed with stirring the time as 20~30min.
The beneficial effects of the invention are as follows：
（1）The present invention is using fir timber as raw material, and incorporation phenol and hexa obtain timber after crushing, grinding mashing
Liquefy wood pulp, and purifying wood pulp is obtained by filtration after Wood liquefied wood pulp is diluted with acetone, by the distillation of purifying wood pulp, dry, high temperature
Charing obtains carbonized woody fiber, and perlite with vitrifying microballon by certain mass ratio is mixed to get and mixes aggregate, by polyethers
Glycol is placed in rosin in three-necked flask, and heating under nitrogen protection is dispersed with stirring, and adds hexamethylene diisocyanate, methylol third
The raw materials such as acid, glycerine and maleic anhydride, are obtained by the reaction polyurethane slurry, and carbonized wooden fiber is mixed into polyurethane slurry, is mixed
Aggregate is closed, obtains toughening leakproof polyurethane grouting material by reacting, being dispersed with stirring, carbonized wooden fiber has by force in the present invention
Strong thickening, enhancing effect, the structural viscosity of carbonized wooden fiber can improve the viscoplasticity of polyurethane grouting material, when pouring number with
The fiber of ten thousand meters is evenly distributed in grouting material, is played the role of good micro- arrangement of reinforcement, is maintained in grouting material steep well
The globality of foam structure makes somewhere stress concentration after mortar molding, energy to failure increase, so as to improve polyurethane grouting material
Toughness；
（2）Maleic anhydride, glycerine react in the generating process of polyurethane with rosin successively in the present invention, and to rosin into
Row is modified, and is primarily due on the double key carbon of maleic anhydride there are two electrophilic carbonyl, therefore maleic anhydride and rosin can be
It being smoothed out reacting under conditions of heating, obtains maleic rosin, maleic rosin increases the degree of functionality of molecule, thus with higher
Softening point, then, maleic rosin and glycerine reaction generate modified rosin resin, and reaction belongs to polyesterification reaction, passes through ester
The acid value of maleic rosin can be reduced by changing reaction, improve its softening point, and improve its stability, the raising of softening point makes injection material
The glass transition temperature of material reduces, and in room temperature aquation, polyurethane grouting material keeps preferable viscoelastic property, and polyurethane fills
Pulp material can be closer with being bonded for building cracks, containing expanded perlite and vitrifying microballon, polyurethane in additional mixing aggregate
After slurry is penetrated into mixing aggregate, thermal expansion coefficients reduce, so as to which polyurethane grouting material be made to be influenced to become by expanding with heat and contract with cold
It is small, possess preferable impervious leakage-stopping function, have a extensive future.
Specific embodiment
Fir timber is placed in 30~45min of crushing in pulverizer, sawdust is obtained, 400~450g sawdusts is placed in mill
In, 600~700mL water is added in into mill, grinding 3~4h of mashing obtains wood pulp, 40~50g phenol, 20 are added in into wood pulp
~25g hexas stir 30~40min under room temperature, stand 4~5h, obtain Wood liquefied wood pulp；To Wood liquefied wood
200~300mL acetone is added in slurry, is filtered after 3~5min of agitation and dilution, removes wooden slag, purifying wood pulp is obtained, wood pulp will be purified
It is placed in the cucurbit with condensing unit, is heated to 100~110 DEG C, distill 4~6h, obtain product of distillation, will distill
Product is placed in baking oven, is heated to 90~100 DEG C, and dry 4~5h obtains wood fibre；Wood fibre is placed in calcining
In stove, stove evacuation will be calcined, be heated to 600~650 DEG C, 3~4h of high temperature carbonization obtains carbonized wooden fiber, by 200
Purpose expanded perlite is that 1 ︰ 3 is mixed in mass ratio with the vitrifying microballon that grain size is 0.1~0.2mm, obtains mixing aggregate；It presses
Parts by weight meter adds in 30~40 parts of polyetherdiol, 20~30 parts of rosin into the dry three-necked flask with condensing unit,
Under nitrogen protection, with the heating rate temperature programming of 3~5 DEG C/min to 90~100 DEG C, and with magnetic stirring apparatus with 200~
The rotating speed of 300r/min is dispersed with stirring 30~40min；Count in parts by weight, into above-mentioned three-necked flask add in 80~90 parts oneself two
Isocyanates, the reaction was continued 2~3h treat that three-necked flask is cooled to 50~60 DEG C, add in 10~15 parts into three-necked flask successively
Dihydromethyl propionic acid, 20~30 parts of glycerine and 20~25 parts of maleic anhydrides, 3~5 parts of dibutyl tin laurates are dissolved in 35~
After 40 parts of acetone, instilled in three-necked flask with the drop rate of 2~3mL/min with constant pressure funnel, heat up, control when being added dropwise
Heating rate processed is 3~5 DEG C/min, is warming up to 80~82 DEG C, and the reaction was continued 3~4h obtains polyurethane slurry；In parts by weight
Meter adds in 12~15 parts of carbonized wooden fibers, 30~40 parts of mixing aggregates into 70~80 parts of polyurethane slurries, 300~
Under the speed of agitator state of 400r/min, continue to add in 0.8~1.0 part of triethylamine into polyurethane slurry, after reacting 5~7min
Speed of agitator is improved to 600~800r/min, 20~30min is dispersed with stirring, obtains toughening leakproof polyurethane grouting material.
Example 1
Fir timber is placed in pulverizer and crushes 30min, obtains sawdust, 400g sawdusts are placed in mill, is added into mill
Enter 600mL water, grinding mashing 3h obtains wood pulp, 40g phenol, 20g hexas are added in into wood pulp, is stirred under room temperature
30min stands 4h, obtains Wood liquefied wood pulp；200mL acetone is added in into Wood liquefied wood pulp, mistake after agitation and dilution 3min
Filter removes wooden slag, obtains purifying wood pulp, and purifying wood pulp is placed in the cucurbit with condensing unit, is heated to 100
DEG C, 4h is distilled, product of distillation is obtained, product of distillation is placed in baking oven, is heated to 90 DEG C, dry 4h obtains wooden fibre
Dimension；Wood fibre is placed in calcining furnace, stove evacuation will be calcined, is heated to 600 DEG C, high temperature carbonization 3h is carbonized
The expanded perlite of 200 mesh with the vitrifying microballon that grain size is 0.1mm is that 1 ︰ 3 is mixed in mass ratio, is mixed by wood fibre
Close aggregate；It counts in parts by weight, 30 parts of polyetherdiol, 20 portions of pines is added in into the dry three-necked flask with condensing unit
Perfume (or spice), under nitrogen protection, with the heating rate temperature programming of 3 DEG C/min to 90 DEG C, and with magnetic stirring apparatus with 200r/min's
Rotating speed is dispersed with stirring 30min；It counts in parts by weight, 80 parts of hexamethylene diisocyanates is added in into above-mentioned three-necked flask, the reaction was continued
2h treats that three-necked flask is cooled to 50 DEG C, adds in 10 parts of dihydromethyl propionic acids, 20 parts of glycerine and 20 portions of horses into three-necked flask successively
Carry out acid anhydrides, after 3 parts of dibutyl tin laurates are dissolved in 35 parts of acetone, with constant pressure funnel with the drop rate of 2mL/min
It instills in three-necked flask, heat up when being added dropwise, control heating rate is 3 DEG C/min, is warming up to 80 DEG C, and the reaction was continued 3h is obtained
Polyurethane slurry；It counts in parts by weight, 12 parts of carbonized wooden fibers, 30 parts of mixing aggregates is added in into 70 parts of polyurethane slurries,
Under the speed of agitator state of 300r/min, continue to add in 0.8 part of triethylamine into polyurethane slurry, improve and stir after reaction 5min
Mix rotating speed is dispersed with stirring 20min, obtains toughening leakproof polyurethane grouting material to 600r/min.
Example 2
Fir timber is placed in pulverizer and crushes 37min, obtains sawdust, 425g sawdusts are placed in mill, is added into mill
Enter 650mL water, grinding mashing 3.5h obtains wood pulp, 45g phenol, 23g hexas are added in into wood pulp, is stirred under room temperature
35min is mixed, 4.5h is stood, obtains Wood liquefied wood pulp；250mL acetone, agitation and dilution 4min are added in into Wood liquefied wood pulp
After filter, remove wooden slag, obtain purifying wood pulp, will purifying wood pulp be placed in the cucurbit with condensing unit, be heated to
105 DEG C, 5h is distilled, product of distillation is obtained, product of distillation is placed in baking oven, be heated to 95 DEG C, dry 4.5h obtains wood
Matter fiber；Wood fibre is placed in calcining furnace, stove evacuation will be calcined, is heated to 625 DEG C, high temperature carbonization 3.5h is obtained
With the vitrifying microballon that grain size is 0.1mm it is that 1 ︰ 3 is mixed in mass ratio by the expanded perlite of 200 mesh to carbonized wooden fiber,
Obtain mixing aggregate；It counts in parts by weight, 35 parts of polyetherdiol, 25 is added in into the dry three-necked flask with condensing unit
Part rosin, under nitrogen protection, with the heating rate temperature programming of 4 DEG C/min to 95 DEG C, and with magnetic stirring apparatus with 250r/
The rotating speed of min is dispersed with stirring 35min；It counts in parts by weight, 85 parts of hexamethylene diisocyanates is added in into above-mentioned three-necked flask, continue
React 2.5h, treat that three-necked flask is cooled to 55 DEG C, successively into three-necked flask add in 13 parts of dihydromethyl propionic acids, 25 parts of glycerine and
23 parts of maleic anhydrides, after 4 parts of dibutyl tin laurates are dissolved in 38 parts of acetone, with constant pressure funnel with 2.5mL/min's
Drop rate is instilled in three-necked flask, is heated up when being added dropwise, control heating rate is 4 DEG C/min, is warming up to 81 DEG C, the reaction was continued
3.5h obtains polyurethane slurry；Count in parts by weight, into 75 parts of polyurethane slurries add in 1. parts of carbonized wooden fibers, 35 parts
Aggregate is mixed, under the speed of agitator state of 350r/min, continues to add in 0.9 part of triethylamine into polyurethane slurry, reaction
Speed of agitator is improved after 6min to 700r/min, 25min is dispersed with stirring, obtains toughening leakproof polyurethane grouting material.
Example 3
Fir timber is placed in pulverizer and crushes 45min, obtains sawdust, 450g sawdusts are placed in mill, is added into mill
Enter 700mL water, grinding mashing 4h obtains wood pulp, 50g phenol, 25g hexas are added in into wood pulp, is stirred under room temperature
40min stands 5h, obtains Wood liquefied wood pulp；300mL acetone is added in into Wood liquefied wood pulp, mistake after agitation and dilution 5min
Filter removes wooden slag, obtains purifying wood pulp, and purifying wood pulp is placed in the cucurbit with condensing unit, is heated to 110
DEG C, 6h is distilled, product of distillation is obtained, product of distillation is placed in baking oven, is heated to 100 DEG C, dry 5h obtains wooden fibre
Dimension；Wood fibre is placed in calcining furnace, stove evacuation will be calcined, is heated to 650 DEG C, high temperature carbonization 4h is carbonized
The expanded perlite of 200 mesh with the vitrifying microballon that grain size is 0.2mm is that 1 ︰ 3 is mixed in mass ratio, is mixed by wood fibre
Close aggregate；It counts in parts by weight, 40 parts of polyetherdiol, 30 portions of pines is added in into the dry three-necked flask with condensing unit
Perfume (or spice), under nitrogen protection, with the heating rate temperature programming of 5 DEG C/min to 100 DEG C, and with magnetic stirring apparatus with 300r/min's
Rotating speed is dispersed with stirring 40min；It counts in parts by weight, 90 parts of hexamethylene diisocyanates is added in into above-mentioned three-necked flask, the reaction was continued
3h treats that three-necked flask is cooled to 60 DEG C, adds in 15 parts of dihydromethyl propionic acids, 30 parts of glycerine and 25 portions of horses into three-necked flask successively
Carry out acid anhydrides, after 5 parts of dibutyl tin laurates are dissolved in 40 parts of acetone, with constant pressure funnel with the drop rate of 3mL/min
It instills in three-necked flask, heat up when being added dropwise, control heating rate is 5 DEG C/min, is warming up to 82 DEG C, and the reaction was continued 4h is obtained
Polyurethane slurry；It counts in parts by weight, 15 parts of carbonized wooden fibers, 40 parts of mixing aggregates is added in into 80 parts of polyurethane slurries,
Under the speed of agitator state of 400r/min, continue to add in 1.0 parts of triethylamines into polyurethane slurry, improve and stir after reaction 7min
Mix rotating speed is dispersed with stirring 30min, obtains toughening leakproof polyurethane grouting material to 800r/min.
Comparative example
With the polyurethane grouting material of company of Beijing production as a comparison case
Polyurethane grouting material in toughening leakproof polyurethane grouting material produced by the present invention and comparative example is detected, is examined
The results are shown in Table 1 for survey：
1st, test method
Compression strength is with reference to GB/T2567-2008 standard tests.
Size is made as 100mm × 100mm × 500mm test specimens in example 1~3 and comparative example prepared by the present invention,
Test specimen is moved in standard curing room rapidly after pouring and is conserved, coefficient of thermal expansion is measured when conserving to 28 days.
Table 1
| Test event | Example 1 | Example 2 | Example 3 | Comparative example |
| Compression strength（MPa） | 112 | 118 | 123 | 85 |
| Tensile strength（MPa） | 55 | 59 | 67 | 38 |
| Elongation at break（%） | 15.4 | 15.7 | 16.0 | 10.6 |
| Impermeability pressure（MPa） | 3.24 | 3.32 | 3.41 | 2.31 |
| Impermeability pressure ratio（%） | 514 | 526 | 537 | 452 |
| Coefficient of thermal expansion（×10-6/℃） | 11.3 | 10.9 | 10.7 | 15.8 |
From the data in table 1, it can be seen that toughening leakproof polyurethane grouting material produced by the present invention, good mechanical properties, toughness is strong, not
With being not susceptible to deformation in environment, and antiseep effect is good, hence it is evident that better than comparative example product.Therefore, before there is wide use
Scape.
Claims (7)
1. a kind of preparation method of toughening leakproof polyurethane grouting material, it is characterised in that specifically preparation process is：
（1）Fir timber is placed in pulverizer and is crushed, obtains sawdust, 400~450g sawdusts are placed in mill, to mill
Middle addition 600~700mL water, grinding mashing obtain wood pulp, 40~50g phenol, 20~25g hexa-methylenes are added in into wood pulp
Tetramine is stirred under room temperature, is stood, is obtained Wood liquefied wood pulp；
（2）200~300mL acetone is added in into Wood liquefied wood pulp, is filtered after agitation and dilution, removes wooden slag, obtains purifying wood
Slurry, purifying wood pulp is placed in the cucurbit with condensing unit, heat temperature raising, and distillation obtains product of distillation, by product of distillation
It is placed in baking oven, heat temperature raising, it is dry, obtain wood fibre；
（3）Wood fibre is placed in calcining furnace, stove evacuation, heat temperature raising will be calcined, high temperature carbonization obtains carbonized wooden fibre
Dimension, expanded perlite is mixed with vitrifying microballon, obtains mixing aggregate；（4）It counts in parts by weight, to dry with condensation
30~40 parts of polyetherdiol, 20~30 parts of rosin are added in the three-necked flask of device, under nitrogen protection, temperature programming is used in combination
Magnetic stirrer is disperseed；
（5）It counts in parts by weight, 80~90 parts of hexamethylene diisocyanates is added in into above-mentioned three-necked flask, the reaction was continued, treats three mouthfuls
Flask cools down, and adds in 10~15 parts of dihydromethyl propionic acids, 20~30 parts of glycerine and 20~25 parts of Malaysias into three-necked flask successively
Acid anhydrides after 3~5 parts of dibutyl tin laurates are dissolved in 35~40 parts of acetone, is instilled with constant pressure funnel in three-necked flask,
It heats up when being added dropwise, the reaction was continued, obtains polyurethane slurry；
（6）Count in parts by weight, added in into 70~80 parts of polyurethane slurries 12~15 parts of carbonized wooden fibers, 30~40 parts it is mixed
Aggregate is closed, under stirring, continues to add in 0.8~1.0 part of triethylamine into polyurethane slurry, stirring is improved after reaction and is turned
Speed is dispersed with stirring, and obtains toughening leakproof polyurethane grouting material.
2. a kind of preparation method of toughening leakproof polyurethane grouting material according to claim 1, it is characterised in that：
Step（1）The grinding time is 30~45min, and grinding beating time is 3~4h, and mixing time is 30~40min,
Time of repose is 4~5h.
3. a kind of preparation method of toughening leakproof polyurethane grouting material according to claim 1, it is characterised in that：
Step（2）The agitation and dilution time is 3~5min, and temperature is 100~110 DEG C after heat temperature raising, distillation time 4
~6h, temperature is 90~100 DEG C after heat temperature raising, and drying time is 4~5h.
4. a kind of preparation method of toughening leakproof polyurethane grouting material according to claim 1, it is characterised in that：
Step（3）Temperature is 600~650 DEG C after the heat temperature raising, and the high temperature carbonization time is 3~4h, expanded perlite
Grain size is 200 mesh, and the grain size of vitrifying microballon is 0.1~0.2mm, and expanded perlite is with the mass ratio that vitrifying microballon mixes
1 ︰ 3.
5. a kind of preparation method of toughening leakproof polyurethane grouting material according to claim 1, it is characterised in that：Step
（4）The heating rate is 3~5 DEG C/min, and temperature is 90~100 DEG C after heating, magnetic stirring apparatus rotating speed for 200~
300r/min is dispersed with stirring the time as 30~40min.
6. a kind of preparation method of toughening leakproof polyurethane grouting material according to claim 1, it is characterised in that：
Step（5）The reaction was continued time is 2~3h, and temperature is 50~60 DEG C after three-necked flask cooling, drop rate 2
~3mL/min, control heating rate are 3~5 DEG C/min, and temperature is 80~82 DEG C after heating, and the reaction was continued, and the time is 3~4h.
7. a kind of preparation method of toughening leakproof polyurethane grouting material according to claim 1, it is characterised in that：
Step（6）The speed of agitator is 300~400r/min, and the reaction time is 5~7min, improves rotating speed after speed of agitator
For 600~800r/min, the time is dispersed with stirring as 20~30min.
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| CN108975823A (en) * | 2018-08-31 | 2018-12-11 | 史茜赟 | A kind of preparation method of low-shrinkage and high-strength degree joint trimming agent |
| CN109206582A (en) * | 2018-08-14 | 2019-01-15 | 山东科技大学 | A kind of compound high polymer of double aggregates and its grouting method and application |
| CN113463485A (en) * | 2021-07-14 | 2021-10-01 | 深圳市粤通建设工程有限公司 | Composite grouting material construction method |
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| US20170121918A1 (en) * | 2015-10-14 | 2017-05-04 | Heeron Tech(Wuhan)New Materials Co., Ltd. | Epoxy mortar adapted in bridge expansion joint and construction method thereof |
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| CN101135075A (en) * | 2007-10-11 | 2008-03-05 | 北京林业大学 | Wood liquefied carbide fiber, protofilament and preparation method thereof |
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| CN109206582A (en) * | 2018-08-14 | 2019-01-15 | 山东科技大学 | A kind of compound high polymer of double aggregates and its grouting method and application |
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| CN113463485A (en) * | 2021-07-14 | 2021-10-01 | 深圳市粤通建设工程有限公司 | Composite grouting material construction method |
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