CN112143216A - Polyurethane grouting reinforcement material and preparation method thereof - Google Patents
Polyurethane grouting reinforcement material and preparation method thereof Download PDFInfo
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- 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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0095—Mixtures of at least two compounding ingredients belonging to different one-dot groups
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
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- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/101—Esters; Ether-esters of monocarboxylic acids
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
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- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
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- C08L75/06—Polyurethanes from polyesters
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
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- C09K5/14—Solid materials, e.g. powdery or granular
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
- C08J2375/06—Polyurethanes from polyesters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
- C08J2375/08—Polyurethanes from polyethers
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Abstract
The invention provides a polyurethane grouting reinforcement material and a preparation method thereof, which can obviously reduce the reaction temperature of the polyurethane reinforcement material in the curing process on the basis of not influencing the performance of the original polyurethane grouting reinforcement material; the preparation method of the polyurethane grouting reinforcement material provided by the invention is simple, safe and environment-friendly, is easy to realize industrialization, and has a wide development prospect.
Description
Technical Field
The invention belongs to the technical field of grouting reinforcement, and particularly relates to a polyurethane grouting reinforcement material and a preparation method thereof.
Background
The polyurethane grouting reinforcement material is widely used for reinforcing coal rock mass due to good mechanical property, curing time, weather resistance and adjustable viscosity. However, the polyurethane is exothermic in the curing process, and heat accumulation is easily generated if the heat accumulation is not controlled, so that the local temperature rise is rapid, and particularly, safety accidents are easily caused in the special environment under a coal mine. Aiming at the safety accidents caused by frequent frequency such as spontaneous combustion, core burning and the like caused by rapid heat storage due to more heat release in the use process of the existing polyurethane grouting material. The new industry standard AQ 1089-2011 being modified puts new requirements on organic based reinforcement materials: the highest reaction temperature is lower than 100 ℃, and the compressive strength is not lower than 40 MPa. Therefore, it is highly desirable to develop a low heat accumulation polyurethane grouting reinforcement material that can reduce the maximum reaction temperature of the material and ensure the strength performance of the material.
The phase-change material can absorb/emit heat when the temperature difference exists between the environment and the phase-change material, the temperature of the material is almost kept unchanged, and the phase-change material is widely applied to the fields of spaceflight, buildings, clothes, refrigeration equipment and the like. The organic phase change material is one of the organic phase change materials, and has the advantages of good solid forming, difficult phase separation and supercooling, small corrosivity, stable performance and the like. However, the organic material also has the problems of low thermal conductivity, easy leakage during phase change and the like, and the organic material is compounded with the carbon material to make up for the defects and obtain the phase change energy storage material with better performance and more suitable for application. By utilizing the characteristics of the phase-change material and the carbon material, the two materials are compounded and are introduced into the polyurethane reinforcing material as a constant-temperature additive, so that a new idea is provided for reducing the reaction heat storage of the polyurethane reinforcing material.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a polyurethane grouting reinforcement material and a preparation method thereof; the method aims to remarkably reduce the reaction temperature of the polyurethane reinforcing material in the curing process on the basis of not influencing the performance of the original polyurethane grouting reinforcing material, thereby avoiding the occurrence of fire caused by local overheating.
In order to achieve the purpose, the invention provides the following technical scheme: the polyurethane grouting reinforcement material comprises a component A and a component B, wherein the component A comprises the following substances in parts by weight:
the component B comprises the following substances in parts by weight:
40-80 parts of polyisocyanate
5-20 parts of diluent
Further, the constant temperature additive comprises 60-80 parts by weight of an organic phase change energy storage material and 20-40 parts by weight of a heat conduction carbon material, and the organic phase change energy storage material and the heat conduction carbon material are mixed and ground, and the constant temperature additive is obtained after cooling to room temperature.
Further, the organic phase change energy storage material is at least one of chlorinated polyethylene, polyvinyl alcohol, polyethylene glycol, paraffin, stearic acid, butyl stearate, palmitic acid and monopalmitin; the heat-conducting carbon material is at least one of carbon black, graphene and carbon nano tubes;
further, the grinding time is 0.5-2 h.
Further, the polymer polyol comprises at least one of polyether polyol and polyester polyol; the flame retardant comprises at least one of tris (2-chloroethyl) phosphate, tris (chloroisopropyl) phosphate, tris (1, 3-dichloro-2-propyl) phosphate, dimethyl methylphosphonate and triphenyl phosphate; the diluent is at least one of dibutyl phthalate, dioctyl phthalate, diisononyl phthalate, tributyl phosphate and chlorinated paraffin.
Further, the catalyst is a compound catalyst of amines and organic tin, wherein the amine catalyst is at least one of triethylene diamine, pentamethyl diethylene triamine, N-methyl piperazine, N, N-2 methyl piperazine, triethanolamine, pyridine and N, N' -dimethyl pyridine, and the organic tin catalyst is at least one of dibutyltin dilaurate, stannous octoate and dibutyltin didodecyl sulfide.
Further, the foam stabilizer is modified silicone oil; the polyisocyanate is polymethylene polyphenyl polyisocyanate.
The invention also provides a preparation method of the polyurethane grouting reinforcement material, which comprises the following specific steps:
s1: preparation of component A: adding polymer polyol into a reaction kettle, heating, dehydrating under a vacuum condition, cooling, sequentially adding a constant-temperature additive, a flame retardant, a catalyst and a foam stabilizer, and uniformly stirring to obtain the component A.
S2: preparation of the component B: adding the polyisocyanate and the diluent into a reaction kettle, and fully mixing to obtain the component B.
S3: mixing A, B components in a volume ratio of 1:1, uniformly mixing to obtain the polyurethane grouting reinforcement material.
Further, in step S1, the temperature in the reaction kettle is 100-120 ℃, the vacuum degree is less than or equal to 0.1Mpa, the stirring is continued for 2-4 h, and the dehydration is carried out after the stirring is finished until the water content is less than 0.05 wt%; in step S1, the mixture is added with constant temperature additive, flame retardant, catalyst and foam stabilizer and then stirred for 0.5-4 h.
Furthermore, when the reinforcing material is used, A, B components are mixed and then are quickly injected into a part needing to be reinforced, and the polyurethane grouting reinforcing material can be quickly solidified in a gel manner, so that the reinforcing effect is achieved.
Compared with the prior art, the invention has at least the following beneficial effects:
the low-temperature polyurethane grouting reinforcement material obtained by the invention has the advantages of less reaction heat release and low maximum reaction temperature, and the purpose of reducing the reaction temperature of the polyurethane material for coal mine reinforcement is achieved by using the constant-temperature additive, so that the problem of fire caused by local overheating is avoided.
The constant temperature additive prepared by the invention consists of an organic phase change material and a carbon material, wherein the organic phase change material can generate solid-liquid phase transition when the temperature of a system reaches a phase change temperature, absorbs heat and hardly changes the temperature; the carbon material is used as a carrier of the organic phase change energy storage material on one hand, and provides high heat conduction property on the other hand, so that the defect of poor heat conduction of the phase change material is overcome. The combination of the two components enables the constant temperature additive to have the characteristics of self-heat absorption, high energy storage and high heat conduction. The constant temperature additive is added into the polyurethane grouting material, so that heat can be absorbed and reduced when the polyurethane is cured and released, and the heat is slowly released when the temperature of the system is reduced to be below the phase change temperature, so that the rapid temperature rise caused by the rapid curing reaction and concentrated heat release of the polyurethane is avoided; on the other hand, the constant temperature additive has good thermal conductivity, and can improve the defect of poor thermal conductivity of the polyurethane material, so that heat generated by curing reaction is quickly led out, and the safety problem caused by thermal runaway due to local heat accumulation is avoided.
Detailed Description
The present invention is further illustrated by the following examples, which are provided for the purpose of clarity and are not intended to limit the scope of the invention.
The components in the following examples are in parts by weight.
Example 1
Preparation of the constant temperature additive: and weighing 80 parts of paraffin and 20 parts of graphene, putting the paraffin and the graphene into a mortar, fully grinding for 2 hours, and cooling to room temperature to obtain the graphene material.
Preparation of component A: adding 40 parts of a mixture of polyether polyol and polyester polyol into a reaction kettle, continuously stirring for 2 hours at 100 ℃ and under the vacuum degree of 0.1MPa, dehydrating until the water content is less than 0.05 wt%, cooling to room temperature, sequentially adding 10 parts of the prepared constant-temperature additive, 5 parts of dimethyl methylphosphonate serving as a flame retardant, 0.5 part of dibutyltin dilaurate, a triethylene diamine and N, N-2 methylpiperazine compound catalyst and 0.5 part of modified silicone oil under a stirring state, and stirring for 0.5 hour to obtain the component A.
Preparation of the component B: adding 40 parts of polymethylene polyphenyl polyisocyanate and 5 parts of dibutyl phthalate into a reaction kettle under a stirring state, and fully mixing to obtain a component B.
Mixing A, B components in a volume ratio of 1:1, mixing them uniformly, pouring them into a mould with diameter of 5cm and height of 10cm, measuring their temperature by thermocouple, and making the maximum reaction temperature be 96.7 deg.C.
The compression performance of the material is tested according to GB/t 2567-2008, and the compression strength is 42.3 MPa.
Example 2
Preparation of the constant temperature additive: and weighing 70 parts of a mixture of butyl stearate and monopalmitin and 30 parts of a mixture of carbon black and graphene, putting the mixture into a mortar, fully grinding for 1.5 hours, and cooling to room temperature to obtain the carbon black/graphene composite material.
Preparation of component A: adding 60 parts of polyester polyol into a reaction kettle, continuously stirring for 4 hours at 110 ℃ and under the vacuum degree of 0.1MPa, dehydrating until the water content is less than 0.05 wt%, cooling to room temperature, sequentially adding 20 parts of the prepared constant-temperature additive, 20 parts of tris (chloroisopropyl) phosphate, 3 parts of a compound catalyst of stannous octoate and N-methylpiperazine and 3 parts of modified silicone oil under stirring, adding 0.5 part of foam stabilizer modified silicone oil, and stirring for 0.5 hour to obtain the component A.
Preparation of the component B: 60 parts of polymethylene polyphenyl polyisocyanate and 10 parts of dioctyl phthalate and diisononyl phthalate mixed diluent are respectively added into a reaction kettle and fully mixed to obtain the component B.
Mixing A, B components in a volume ratio of 1:1, mixing them uniformly, pouring them into a mould with diameter of 5cm and height of 10cm, measuring their temperature by thermocouple, and making the maximum reaction temperature be 96.8 deg.C.
The compression performance of the material is tested according to GB/t 2567-2008, and the compression strength is 42.0 MPa.
Example 3
Preparation of the constant temperature additive: weighing 60 parts of mixture of the palmitic acid and the stearic acid and 40 parts of the heat-conducting carbon material carbon nano tube, placing the mixture and the heat-conducting carbon material carbon nano tube in a mortar, fully grinding for 0.5h, and cooling to room temperature to obtain the constant-temperature additive, wherein the ratio of the palmitic acid to the stearic acid is 1: 2.
Preparation of component A: adding 50 parts of polyether polyol into a reaction kettle, continuously stirring for 4 hours at 120 ℃ and under the vacuum degree of 0.1MPa, dehydrating until the water content is less than 0.05 wt%, cooling to room temperature, sequentially adding 30 parts of the prepared constant-temperature additive, 10 parts of a mixed flame retardant of tris (2-chloroethyl) phosphate and tris (1, 3-dichloro-2-propyl) phosphate, 1 part of di-dodecyl-sulfur-dibutyl-tin, a pentamethyl-diethylenetriamine and pyridine compound catalyst and 2 parts of modified silicone oil under a stirring state, and stirring for 4 hours to obtain the component A.
Preparation of the component B: 80 parts of polymethylene polyphenyl polyisocyanate and 20 parts of chlorinated paraffin and tributyl phosphate mixed diluent are respectively added into a reaction kettle, and the component B can be obtained after full mixing.
Mixing A, B components in a volume ratio of 1:1, mixing them uniformly, pouring them into a mould with diameter of 5cm and height of 10cm, measuring their temperature by thermocouple, and making the maximum reaction temperature be 95.3 deg.C.
The compression performance of the material is tested according to GB/t 2567-2008, and the compression strength is 40.9 MPa.
Example 4
Preparation of the constant temperature additive: weighing 70 parts of a mixture of polyvinyl chloride, polyvinyl alcohol and polyethylene glycol and 30 parts of carbon nano tubes, putting the mixture and the carbon nano tubes into a mortar, fully grinding for 1h, and cooling to room temperature to obtain the constant-temperature additive, wherein the ratio of the polyvinyl chloride to the polyvinyl alcohol to the polyethylene glycol is 1:1: 2.
Preparation of component A: adding 50 parts of polyether polyol into a reaction kettle, continuously stirring for 4 hours at 120 ℃ and under the vacuum degree of 0.1MPa, dehydrating until the water content is less than 0.05 wt%, cooling to room temperature, sequentially adding 30 parts of the prepared constant-temperature additive, 10 parts of the prepared mixed flame retardant of tris (2-chloroethyl) phosphate and triphenyl phosphate, 3 parts of triethanolamine, N-dimethylpyridine, stannous octoate and dibutyltin dilaurate compounded catalyst and 2 parts of modified silicone oil under a stirring state, and stirring for 4 hours to obtain the component A.
Preparation of the component B: 80 parts of polymethylene polyphenyl polyisocyanate and 20 parts of dibutyl phthalate are respectively added into a reaction kettle and fully mixed to obtain the component B.
Mixing A, B components in a volume ratio of 1:1, mixing uniformly, pouring into a mould with the diameter of 5cm and the height of 10cm, measuring the temperature by using a thermocouple, and keeping the maximum reaction temperature at 97.5 ℃.
The compression performance of the material is tested according to GB/t 2567-2008, and the compression strength is 43.1 MPa. The embodiment shows that the polyurethane grouting material prepared by the invention has lower reaction temperature (the highest reaction temperature is lower than 100 ℃) and higher compression strength (higher than 40MPa), compared with the polyurethane reinforcing material adopted at the present stage (the highest temperature is lower than 140 ℃), the reaction temperature is obviously reduced, the strength can meet the requirements of new industrial standards, and the safety application of the polyurethane grouting reinforcing material in coal mines is guaranteed.
The constant-temperature additive is simple in preparation method, wide in raw material source, safe and environment-friendly, does not generate toxic and harmful substances in the preparation and use processes, is easy to realize industrialization, and has wide development prospect.
Claims (10)
1. The polyurethane grouting reinforcement material is characterized by comprising a component A and a component B, wherein the component A comprises the following substances in parts by weight:
the component B comprises the following substances in parts by weight:
40-80 parts of polyisocyanate
And 5-20 parts of a diluent.
2. The polyurethane grouting reinforcement material as claimed in claim 1, wherein the constant temperature additive comprises 60-80 parts by weight of organic phase change energy storage material and 20-40 parts by weight of heat conductive carbon material, and the constant temperature additive is obtained by mixing and grinding the organic phase change energy storage material and the heat conductive carbon material and cooling to room temperature.
3. The polyurethane grouting reinforcement material as claimed in claim 2, wherein the organic phase change energy storage material is at least one of chlorinated polyethylene, polyvinyl alcohol, polyethylene glycol, paraffin, stearic acid, butyl stearate, palmitic acid, and monopalmitin; the heat-conducting carbon material is at least one of carbon black, graphene and carbon nano tubes.
4. The polyurethane grouting reinforcement material as claimed in claim 2, wherein the grinding time is 0.5-2 h.
5. The polyurethane grouting reinforcement material as claimed in claim 1, wherein the polymer polyol includes at least one of polyether polyol and polyester polyol; the flame retardant comprises at least one of tris (2-chloroethyl) phosphate, tris (chloroisopropyl) phosphate, tris (1, 3-dichloro-2-propyl) phosphate, dimethyl methylphosphonate and triphenyl phosphate; the diluent is at least one of dibutyl phthalate, dioctyl phthalate, diisononyl phthalate, tributyl phosphate and chlorinated paraffin.
6. The polyurethane grouting reinforcement material as claimed in claim 1, wherein the catalyst is a compound catalyst of amine and organic tin, wherein the amine catalyst is at least one of triethylene diamine, pentamethyl diethylene triamine, N-methyl piperazine, N-2 methyl piperazine, triethanolamine, pyridine, and N, N' -dimethyl pyridine, and the organic tin catalyst is at least one of dibutyltin dilaurate, stannous octoate, and dibutyltin didodecyl sulfide.
7. The polyurethane grouting reinforcement material as claimed in claim 1, wherein the foam stabilizer is modified silicone oil; the polyisocyanate is polymethylene polyphenyl polyisocyanate.
8. The preparation method of the polyurethane grouting reinforcement material according to any one of claims 1 to 7, characterized by comprising the following steps:
s1: preparation of component A: adding polymer polyol into a reaction kettle, heating, dehydrating under a vacuum condition, cooling, sequentially adding a constant-temperature additive, a flame retardant, a catalyst and a foam stabilizer, and uniformly stirring to obtain a component A;
s2: preparation of the component B: adding polyisocyanate and a diluent into a reaction kettle, and fully mixing to obtain a component B;
s3: mixing A, B components in a volume ratio of 1:1, uniformly mixing to obtain the polyurethane grouting reinforcement material.
9. The preparation method of the polyurethane grouting reinforcement material as claimed in claim 8, wherein in step S1, the temperature in the reaction kettle is 100 ℃ to 120 ℃, the vacuum degree is less than or equal to 0.1Mpa, the stirring is continued for 2h to 4h, and the dehydration is carried out until the moisture content is less than 0.05 wt% after the stirring is completed; in step S1, the mixture is added with constant temperature additive, flame retardant, catalyst and foam stabilizer and then stirred for 0.5-4 h.
10. The method for preparing the polyurethane grouting reinforcement material as claimed in claim 8, wherein in use, A, B components are mixed and then rapidly injected into a part to be reinforced, and the polyurethane grouting reinforcement material can be rapidly solidified by gel to play a reinforcement role.
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Cited By (5)
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| CN115368059A (en) * | 2022-09-20 | 2022-11-22 | 广州大学 | Tunnel synchronous grouting shock insulation material and application thereof |
| CN115505090A (en) * | 2022-10-13 | 2022-12-23 | 万华节能科技(烟台)有限公司 | Low-temperature reaction type polyurethane composite heat-insulating material and preparation method thereof |
| CN116284645A (en) * | 2021-12-20 | 2023-06-23 | 煤炭科学技术研究院有限公司 | Safe composite grouting reinforcement material with heat conduction function and preparation method |
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| CN116284645A (en) * | 2021-12-20 | 2023-06-23 | 煤炭科学技术研究院有限公司 | Safe composite grouting reinforcement material with heat conduction function and preparation method |
| CN116284645B (en) * | 2021-12-20 | 2024-05-07 | 煤炭科学技术研究院有限公司 | Safe composite grouting reinforcement material with heat conduction function and preparation method |
| CN115181241A (en) * | 2022-08-26 | 2022-10-14 | 河北浩威旭光新材料科技有限公司 | Organic polymer ultralow-temperature reinforcing material for coal rock mass |
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Application publication date: 20201229 |