CN112142950A - High-performance coal mine reinforcing material and preparation method thereof - Google Patents
High-performance coal mine reinforcing material and preparation method thereof Download PDFInfo
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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
- C08G18/77—Polyisocyanates or polyisothiocyanates having heteroatoms in addition to the isocyanate or isothiocyanate nitrogen and oxygen or sulfur
- C08G18/78—Nitrogen
- C08G18/79—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates
- C08G18/791—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates containing isocyanurate groups
- C08G18/794—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates containing isocyanurate groups formed by oligomerisation of aromatic isocyanates or isothiocyanates
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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
- C08G18/3206—Polyhydroxy compounds aliphatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
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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
- 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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- 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
- 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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- 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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5317—Phosphonic compounds, e.g. R—P(:O)(OR')2
- C08K5/5333—Esters of phosphonic acids
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Abstract
The invention belongs to the technical field of coal mine reinforcing materials, and relates to a high-performance coal mine reinforcing material and a preparation method thereof. The material is prepared from a component A and a component B according to the volume ratio of 1: 1. Wherein the component A adopts polyether polyol as a main agent and comprises 70-90 parts of polyether polyol, 5-20 parts of flame retardant, 0.5-3 parts of catalyst and 1-10 parts of auxiliary agent. The component B adopts polyisocyanate as a main agent and comprises 70-100 parts of polymeric MDI and 0-30 parts of flame retardant. The invention has the advantages that: (1) the invention has high mechanical strength of materials through the formula design, and can obviously improve the overall safety of the soft and broken coal rock stratum; (2) the material is uniform liquid, the grouting effect cannot be influenced by precipitation and delamination of solid components, and the material does not release harmful substances such as formaldehyde and the like; (3) the vegetable oil ester in the auxiliary agent is from renewable vegetable oil, so that the consumption of petroleum resources is reduced, the auxiliary agent has the advantages of energy conservation and emission reduction, and the vegetable oil ester and the flame retardant have a synergistic effect and are beneficial to flame retardant performance and mechanical performance.
Description
Technical Field
The invention belongs to the technical field of coal mine reinforcing materials, and particularly relates to a high-performance coal mine reinforcing material and a preparation method thereof.
Background
Coal is in a very important basic position in the primary energy production and consumption structure of China, and is expected to account for more than 50% by 2050. Along with the expansion of the coal mining scale, the coal mining environment is increasingly complex and worsened, various coal mine accidents occur sometimes, and the coal mine roof accident is always a major hidden danger in the coal mine safety production. In the production process of coal mines, generally, the grouting reinforcement is carried out on faults, broken zone joints, weak interlayers and the like in the excavation roadway to avoid the separation of roof strata and even roof fall. Therefore, the reliability of the grouting reinforcement material is the primary requirement in coal mine safety production. The reinforcing materials of urea formaldehyde and phenol aldehyde in the most applied organic polymer grouting reinforcing materials at present have the advantages of good permeability, adjustable gel speed, low cost and the like, but the use of the reinforcing materials is limited by the characteristics of low strength, brittleness and the like of the materials; in addition, harmful substances such as formaldehyde existing in the material are released, so that the application of the underground coal mine in a closed narrow space is further limited, and the material cannot be widely recognized.
In recent years, many fire accidents happen, so that the research of the industry focuses on the exothermicity and the flame retardance, but some materials contain solid components, and the grouting proportion is influenced by the precipitation and the delamination of the material components, so that the grouting effect is influenced. Some reinforcing materials achieve better exothermicity, but sacrifice the mechanical properties of the material. Therefore, pursuit of a certain property of the material on one side affects the mechanical property and application effect of the material, and can bring new hidden trouble to the safety production of the coal mine.
Therefore, the field expects to develop a reinforcing material with good comprehensive properties of bonding strength, tensile strength, compressive strength and flame retardant property, so as to ensure the safe production of the complex mining environment of the coal mine. In addition, with the consideration of coal mining cost, development of low-cost coal mine reinforcing materials is also a trend. The above is also the motivation direction for the development of coal mine reinforcing materials.
Disclosure of Invention
The invention aims to realize the high reliability of the coal mine reinforcing material through the optimized design, and provides a safe, efficient, environment-friendly and cheap technical approach for coal mining. The invention has the other effect that the auxiliary agent vegetable oil ester is selected, and has the outstanding characteristics of energy conservation, environmental protection and reliable performance due to the synergistic effect with the flame retardant.
The high-performance coal mine reinforcing material comprises the following components:
the high-performance coal mine reinforcing material is prepared from a component A and a component B according to the volume ratio of 1: 1. Wherein:
the component A consists of 70-90 parts of polyether polyol, 5-20 parts of flame retardant, 0.5-3 parts of catalyst and 1-10 parts of auxiliary agent, and preferably the component A consists of 100 parts by mass;
the component B consists of 70-100 parts of polymeric MDI and 0-30 parts of flame retardant, and the component B preferably accounts for 100 parts by mass;
the isocyanate index R of the high-performance coal mine reinforcing material is 1.0-1.5, and preferably 1.1-1.3.
The polyether polyol is one or a mixture of several, preferably one or several of polyether polyols with 2-6 functionality and molecular weight of 300-1000.
The flame retardant is one or more of tris (2-chloroethyl) phosphate, tris (2-chloropropyl) phosphate, dimethyl methylphosphonate and diethyl ethylphosphonate, and is preferably tris (2-chloropropyl) phosphate.
The catalyst is one or two of an amine catalyst and an organic tin catalyst;
the amine catalyst is one or more of triethylene diamine, N, N-dimethyl cyclohexylamine, N, N, N, N-pentamethyl diethylene triamine and triethanolamine; the organic tin catalyst is selected from stannous octoate or dibutyltin dilaurate;
the auxiliary agent comprises a stabilizer and a plasticizer. Wherein the stabilizer is selected from silicone oil and Tween series products, and accounts for 0.5-4 parts; the plasticizer is from renewable vegetable oil and accounts for 0.5-6 parts; such as synthetic vegetable oil ester plasticizers derived from vegetable oils such as soybean oil, palm oil, corn oil, sunflower oil, and the like. Preferably, the plasticizer is methyl chlorinated palm oil.
The polymeric MDI is a brown liquid and has an-NCO content of 30-32%.
The invention relates to a preparation method of a high-performance coal mine reinforcing material, which comprises the following steps:
1) preparing a component A: adding accurately weighed polyether polyol and flame retardant into a reaction kettle, uniformly stirring, then adding weighed catalyst and auxiliary agent, stirring for 10-60 min, uniformly mixing and barreling.
2) Preparing a component B: accurately weighed polymeric MDI and flame retardant are put into a reaction kettle, stirred for 10min-60min and uniformly mixed to be barreled.
The high-performance coal mine reinforcing material is characterized by having good flame retardant property, and having the compressive strength of more than 60MPa, the tensile strength of more than 25MPa and the bonding strength of more than 10 MPa.
Compared with the prior art, the invention has the following advantages: (1) the invention has high mechanical strength of materials through the formula design, and can obviously improve the overall safety of the soft and broken coal rock stratum; (2) the material is uniform liquid, the grouting effect cannot be influenced by precipitation and delamination of solid components, and the material does not release harmful substances such as formaldehyde and the like; (3) the vegetable oil ester in the auxiliary agent is from renewable vegetable oil, so that the consumption of petroleum resources is reduced, the auxiliary agent has the advantages of energy conservation and emission reduction, and the vegetable oil ester and the flame retardant have a synergistic effect and are beneficial to flame retardant performance and mechanical performance.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention in any way.
The invention mainly inspects the compressive strength, the tensile strength and the bonding strength of the reinforcing material, and simultaneously inspects the flame retardant property of the reinforcing material. The performance test is carried out according to AQ1089-2011 Standard regulation of Polymer materials for coal mine reinforced coal rock mass. The results of the mechanical properties of the reinforcing material of the invention are shown in Table 1, and the results of the flame retardant properties are shown in Table 2.
Example 1
Preparation of a component A: 87 parts of polyether polyol 305 (with the functionality of 3 and the molecular weight of 500), 8 parts of tris (2-chloropropyl) phosphate, 1 part of dibutyltin dilaurate, 0.4 part of triethanolamine, 1.6 parts of tween 80 stabilizer and 2 parts of methyl chloropalmitolate plasticizer are weighed.
B, preparation of a component: 80 parts of polymeric MDI (PM200 or M200) and 20 parts of tris (2-chloropropyl) phosphate are weighed, stirred for 10min-60min and mixed uniformly.
A, B components are prepared into a reinforcing material sample according to the equal volume ratio, and the compressive strength, the tensile strength, the bonding strength and the flame retardant property of the reinforcing material are tested according to AQ1089-2011 standard requirements.
Example 2
Preparation of a component A: 67 parts of polyether polyol 303 (functionality of 3, molecular weight of 300), 10 parts of polyether polyol 4110 (functionality of 4, molecular weight of 500), 15 parts of tris (2-chloroethyl) phosphate, 0.8 part of dibutyltin dilaurate, 0.7 part of triethanolamine, 2 parts of silicone oil AK158 stabilizer and 4.5 parts of chlorinated palm oil methyl ester plasticizer were weighed.
B, preparation of a component: 90 parts of polymeric MDI (PM200 or M200) and 10 parts of tris (2-chloropropyl) phosphate are weighed, stirred for 10min-60min and mixed uniformly.
A, B components are prepared into a reinforcing material sample according to the equal volume ratio, and the compressive strength, the tensile strength, the bonding strength and the flame retardant property of the reinforcing material are tested according to AQ1089-2011 standard requirements.
Example 3
Preparation of a component A: 68 parts of polyether polyol 305 (functionality of 3 and molecular weight of 500), 13 parts of polyether polyol NJ6209 (functionality of 4.5 and molecular weight of 670), 11 parts of dimethyl methylphosphonate, 1 part of dibutyltin dilaurate, 2 parts of Tween 80 stabilizer and 5 parts of chlorinated palm oil methyl ester plasticizer are weighed.
B, preparation of a component: 80 parts of polymeric MDI (PM200 or M200) and 20 parts of tris (2-chloropropyl) phosphate are weighed, stirred for 10min-60min and mixed uniformly.
A, B components are prepared into a reinforcing material sample according to the equal volume ratio, and the compressive strength, the tensile strength, the bonding strength and the flame retardant property of the reinforcing material are tested according to AQ1089-2011 standard requirements.
Example 4
Preparation of a component A: 73 parts of polyether polyol NJ6209 (functionality of 4.5 and molecular weight of 670), 23 parts of tris (2-chloropropyl) phosphate, 0.7 part of dibutyltin dilaurate, 0.5 part of triethylene diamine, 0.8 part of AK158 silicone oil stabilizer and 2 parts of methyl chloropalmitolate plasticizer were weighed.
B, preparation of a component: 80 parts of polymeric MDI (PM200 or M200) and 20 parts of tris (2-chloropropyl) phosphate are weighed, stirred for 10min-60min and mixed uniformly.
A, B components are prepared into a reinforcing material sample according to the equal volume ratio, and the compressive strength, the tensile strength, the bonding strength and the flame retardant property of the reinforcing material are tested according to AQ1089-2011 standard requirements.
Example 5
Preparation of a component A: 68 parts of polyether polyol 305 (functionality of 3, molecular weight of 500), 5 parts of polyether polyol 4110 (functionality of 4, molecular weight of 500), 10 parts of polyether polyol NJ6209 (functionality of 4.5, molecular weight of 670), 12 parts of diethyl ethylphosphonate, 0.4 part of stannous octoate, 0.6 part of triethylene diamine, 1.5 parts of silicone oil AK158 stabilizer and 2.5 parts of chlorinated palm oil methyl ester plasticizer are weighed.
B, preparation of a component: weighing 80 parts of polymeric MDI (PM200 or M200) and 20 parts of diethyl ethylphosphonate, stirring for 10-60 min, and mixing uniformly.
A, B components are prepared into a reinforcing material sample according to the equal volume ratio, and the compressive strength, the tensile strength, the bonding strength and the flame retardant property of the reinforcing material are tested according to AQ1089-2011 standard requirements.
TABLE 1 mechanical Properties of coal mine reinforcing Material in units of MPa
| Mechanical properties | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Compressive strength | 76 | 72 | 74 | 75 | 80 |
| Tensile strength | 32 | 25 | 26 | 33 | 35 |
| Adhesive strength | 12.3 | 11.6 | 11.3 | 12.8 | 13.2 |
TABLE 2 flame retardancy test results of coal mine reinforcing materials
The high-performance reinforcing material for coal mines according to the invention, compared with the preparation of reinforcing materials known in the art, shows that: the prepared reinforcing material has high mechanical strength (the standard requires that the compression strength, the tensile strength and the bonding strength are respectively greater than 60MPa, 20MPa and 3MPa), and the overall safety of the soft crushed coal rock stratum can be obviously improved; the material is uniform liquid, the grouting effect cannot be influenced by precipitation and delamination of solid components, and the material does not release harmful substances such as formaldehyde and the like; the vegetable oil ester in the auxiliary agent is from renewable vegetable oil, so that the consumption of petroleum resources is reduced, the auxiliary agent has the advantages of energy conservation and emission reduction, and the vegetable oil ester and the flame retardant have a synergistic effect and are beneficial to flame retardance and mechanical properties.
While the invention has been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that the invention can be practiced without these specific details. It will be apparent to those skilled in the art that many changes and substitutions can be made without departing from the spirit and scope of the invention.
Claims (9)
1. The high-performance coal mine reinforcing material is characterized by being prepared from a component A and a component B according to the volume ratio of 1: 1; wherein:
the component A consists of 70-90 parts of polyether polyol, 5-20 parts of flame retardant, 0.5-3 parts of catalyst and 1-10 parts of auxiliary agent;
the component B consists of 70-100 parts of polymeric MDI and 0-30 parts of flame retardant;
the isocyanate index R of the high-performance coal mine reinforcing material is 1.0-1.5, and preferably 1.1-1.3.
2. The high-performance coal mine reinforcing material as claimed in claim 1, wherein the polyether polyol is one or more of a mixture of polyether polyol, preferably polyether polyol with 2-6 functionality and molecular weight of 300-1000.
3. A high-performance coal mine reinforcing material according to claim 1, wherein the flame retardant is one or more of tris (2-chloroethyl) phosphate, tris (2-chloropropyl) phosphate, dimethyl methylphosphonate and diethyl ethylphosphonate, and is preferably tris (2-chloropropyl) phosphate.
4. A high performance coal mine reinforcing material according to claim 1, wherein said catalyst is one or both of amine catalyst and organic tin catalyst.
5. The high-performance coal mine reinforcing material is characterized in that the amine catalyst is one or more of triethylene diamine, N, N-dimethyl cyclohexylamine, N, N, N, N-pentamethyl diethylene triamine and triethanolamine; the organic tin catalyst is selected from stannous octoate or dibutyltin dilaurate.
6. A high performance coal mine reinforcing material according to claim 1, wherein said auxiliary agents include stabilizers and plasticizers. Wherein the stabilizer is selected from silicone oil and Tween series products, and accounts for 0.5-4 parts; the plasticizer is from renewable vegetable oil and accounts for 0.5-6 parts; such as synthetic vegetable oil ester plasticizers derived from vegetable oils such as soybean oil, palm oil, corn oil, sunflower oil, and the like. Preferably, the plasticizer is methyl chlorinated palm oil.
7. A high performance coal mine reinforcing material according to claim 1, wherein said polymeric MDI is a brown liquid having-an NCO content of 30% to 32%.
8. The preparation method of the high-performance coal mine reinforcing material according to claim 1, characterized by comprising the following steps:
1) preparing a component A: adding accurately weighed polyether polyol and flame retardant into a reaction kettle, uniformly stirring, then adding weighed catalyst and auxiliary agent, stirring for 10-60 min, uniformly mixing and barreling.
2) Preparing a component B: accurately weighed polymeric MDI and flame retardant are put into a reaction kettle, stirred for 10min-60min and uniformly mixed to be barreled.
9. The high-performance coal mine reinforcing material according to claim 1, wherein the high-performance coal mine reinforcing material has good flame retardant property, and has a compressive strength of more than 60MPa, a tensile strength of more than 25MPa and a bonding strength of more than 10 MPa.
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Cited By (1)
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