CN104277204A - Polyurethane reinforced material for inorganic modified ores and preparation method thereof - Google Patents
Polyurethane reinforced material for inorganic modified ores and preparation method thereof Download PDFInfo
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- 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
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
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- C08K13/02—Organic and inorganic ingredients
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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Abstract
The invention aims at providing a polyurethane reinforced material for inorganic modified ores and a preparation method thereof. The material is prepared by polymerizing components A and B. The component A is prepared from the following substances in percentage by mass: 31-57% of polyether polyol, 10-32% of polyester polyol, 1.0-14% of an inorganic modifier A, 1.0-11% of an inorganic modifier B, 0-1.8% of a foam stabilizer, 1.2-2.0% of a solubilizer, 0-35% of a foaming agent, 0.4-2.6% of a catalyst and 10-30% of a flame retardant; the component B is prepared from the following substances in percentage by mass: 50-75% of polymethylene polyphenyl polyisocyanate, 10-20% of diphenyl-methane-diisocyanate and 10-30% of a compound modifier. By adding the inorganic modifiers and optimizing the formula, the flame retardance of a conventional polyurethane material is improved, the reaction temperature of the material used is greatly reduced, and the potential safety hazard of the material in the using process is eliminated.
Description
Technical field
The invention belongs to polyurethane material field, be specifically related to a kind of inorganic modified mine polyurethane reinforcement material and preparation method thereof.
Background technology
In underground coal mine digging construction process, roof control is the normal key link of producing of safety, and the roof fall that fractured coal and rock causes, wall caving, be the technical barrier that shaft production cannot be avoided always, easy generation falling rocks pounds the accident of people, and therefore tunnel needs reinforcement process.In addition, along with mining depth strengthens, mine inflow increases, and in fractured coal and rock, water content is large, and trickle appears in top board, makes roof control more difficult.According to statistics, smashed to pieces, be rich in water and trickle condition coal and rock accounts for the ratio of stope working surface of coal mines and roadway engineering total amount up to about 30%, in the urgent need to researching and developing one chemical consolidation technology fast and effectively and reinforcement material.
Use traditional polyurethane material in the treatment process of current mine laneway wall, due to shortcomings such as it are inflammable, smoke density is large, temperature of reaction is high, in use there is certain potential safety hazard.
Summary of the invention
The object of this invention is to provide a kind of inorganic modified mine polyurethane reinforcement material, improved the flame retardant properties of conventional urethane material by the optimization adding inorganic modifier and formula; The present invention provides its preparation method simultaneously.
Inorganic modified mine polyurethane reinforcement material of the present invention, is polymerized by component A and B component, wherein:
The raw material of component A, is calculated in mass percent, and proportioning is as follows:
The raw material of B component, is calculated in mass percent, and proportioning is as follows:
Poly methylene poly phenyl poly isocyanate: 50 ~ 75%
'-diphenylmethane diisocyanate: 10 ~ 20%
Composite modifier: 10 ~ 30%
Further, the weight ratio of A, B component is A:B=1:1.
Further, polyether glycol adopts functionality to be 8, and molecular weight is the poly(propylene oxide) ethoxylated polyhydric alcohol of 300 ~ 1000;
Further, polyester polyol adopts functionality to be 2, and molecular weight is the benzoic anhydride polyester polyol of 400 ~ 1000;
Further, inorganic modifier A employing degree Beaume is the potassium silicate aqueous solution of 20 ~ 60 degree;
Further, inorganic modifier B is the superfine powder that a kind of median size be mixed by calcium carbonate, barium sulfate, kaolin and trimeric cyanamide is less than 50 μm, and four kinds of raw materials quality are than being 1:1.5:2:1;
Further, suds-stabilizing agent adopts Si-C class tensio-active agent, is selected from the AK-8872 that Mei Side chemical inc, Jiangsu provides;
Further, solubilizing agent adopts alkylphenol-polyethenoxy base ether nonionic type tensio-active agent, preferred OP-10.
Further, whipping agent adopts the chloro-1-fluoroethane of 1,1-bis-;
Further, catalyzer adopts organo-metallic catalyst and organic amine catalyst; Preferred dibutyl tin laurate, 2,4,6-tri-(dimethylamino methyl) phenol and five methyl diethylentriamines, the mass ratio between three is 0.5 ~ 1.5:1 ~ 2.5:0.5 ~ 2;
Further, fire retardant adopts phosphate ester flame retardants, preferably phosphoric acid trichlorine propyl ester.
Further, composite modifier is mixed by dimethyl phthalate, dibutyl phthalate and dioctyl phthalate (DOP), and three kinds of raw materials quality are than being 1:0-2:1-1.5.
The preparation method of described inorganic modified mine polyurethane reinforcement material comprises the following steps:
(1) component A material is prepared: first stir in load weighted polyether glycol, polyester polyol loading mixing kettle, then load weighted inorganic modifier A, inorganic modifier B, catalyzer, whipping agent, solubilizing agent, suds-stabilizing agent, fire retardant is added, even in stirring at normal temperature, after sampling detection is qualified, get final product barrelling;
(2) B component material is prepared: stir in load weighted poly methylene poly phenyl poly isocyanate, '-diphenylmethane diisocyanate, composite modifier loading mixing kettle, after sampling detection is qualified, get final product barrelling;
(3) A, B component material are mixed by the weight ratio of A:B=1:1, obtain inorganic modified mine polyurethane reinforcement material.
Beneficial effect of the present invention:
(1) flame retardant properties of conventional urethane material can be improve by the optimization adding inorganic modifier and formula, and greatly reduce temperature of reaction when it uses, eliminate its potential safety hazard in use;
(2) material of the present invention is by formulating of recipe, and normal temperature uses curing speed adjustable, and concretion body strength is high, and has fine toughness, can bear mining influence subsequently, and stock liquid viscosity is low good with rock coal body cohesiveness;
(3) material related raw material of the present invention is green, pollution-free, low smell, not containing volatile solvent, does not produce any toxic gas, harmless, meets the use under ore deposit and environmental requirement completely.
After testing, product quality indicator can reach the inorganic modified mine polyurethane reinforcement material that the present invention obtains:
Performance fullys meet the requirement of mining reinforcement material.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
100 kilograms, preparation component A material, weigh respectively: polyether glycol 45 kilograms, polyester polyol 15 kilograms, inorganic modifier A 10 kilograms, inorganic modifier B 5 kilograms, solubilizing agent OP-101.5 kilogram, catalyst dibutyltin dilaurylate 0.625 kilogram, catalyzer 2,4,6-tri-(dimethylamino methyl) phenol 1.25 kilograms, catalyzer five methyl diethylentriamine 0.625 kilogram, fire retardant trichloropropyl phosphate 21 kilograms.Load weighted polyether glycol and polyester polyol are loaded in mixing kettle and stir, then add the inorganic modifier A weighed up respectively, inorganic modifier B, solubilizing agent, catalyzer, fire retardant stirs at normal temperatures, after sampling detection is qualified, gets final product barrelling.
100 kilograms, preparation B component material, weighs: poly methylene poly phenyl poly isocyanate 60 kilograms, '-diphenylmethane diisocyanate 20 kilograms, composite modifier 20 kilograms respectively.
Wherein:
Polyether glycol adopts functionality to be 8, and molecular weight is the poly(propylene oxide) ethoxylated polyhydric alcohol of 500,
Polyester polyol adopts functionality to be 2, and molecular weight is the benzoic anhydride polyester polyol of 600,
Inorganic modifier A employing degree Beaume is the potassium silicate aqueous solution of 20 degree,
Inorganic modifier B is a kind of median size be mixed by calcium carbonate, barium sulfate, kaolin and trimeric cyanamide is the superfine powder of 40um, and four kinds of raw materials quality ratios are 1:1.5:2:1,
Composite modifier is mixed by dimethyl phthalate, dibutyl phthalate and dioctyl phthalate (DOP), and three kinds of raw materials quality are than being 1:1:1.
A, B component material are reacted after pressing the mixing of A:B=100:100 weight proportion, can obtain inorganic modified mine polyurethane reinforcement material, its product quality indicator is as follows:
Embodiment 2
100 kilograms, preparation component A material, weigh respectively: polyether glycol 50 kilograms, polyester polyol 8 kilograms, inorganic modifier A 8 kilograms, inorganic modifier B 3 kilograms, suds-stabilizing agent AK-88721 kilogram, the chloro-1-fluoroethane of whipping agent 1,1-bis-5 kilograms, solubilizing agent OP-101.7 kilogram, catalyst dibutyltin dilaurylate 0.65 kilogram, catalyzer 2,4,6-tri-(dimethylamino methyl) phenol 1.35 kilograms, catalyzer five methyl diethylentriamine 0.6 kilogram, fire retardant trichloropropyl phosphate 20.7 kilograms.Load weighted polyether glycol and polyester polyol are loaded in mixing kettle and stirs, then add the inorganic modifier A weighed up respectively, inorganic modifier B, suds-stabilizing agent, whipping agent, solubilizing agent, catalyzer, fire retardant stirs at normal temperatures, after sampling detection is qualified, gets final product barrelling.
100 kilograms, preparation B component material, weighs: poly methylene poly phenyl poly isocyanate 70 kilograms, '-diphenylmethane diisocyanate 10 kilograms, composite modifier 20 kilograms respectively.
Wherein:
Polyether glycol adopts functionality to be 8, and molecular weight is the poly(propylene oxide) ethoxylated polyhydric alcohol of 800,
Polyester polyol adopts functionality to be 2, and molecular weight is the benzoic anhydride polyester polyol of 750,
Inorganic modifier A employing degree Beaume is the potassium silicate aqueous solution of 40 degree,
Inorganic modifier B is a kind of median size be mixed by calcium carbonate, barium sulfate, kaolin and trimeric cyanamide is the superfine powder of 40um, and four kinds of raw materials quality ratios are 1:1.5:2:1,
Composite modifier is mixed by dimethyl phthalate, dibutyl phthalate and dioctyl phthalate (DOP), and three kinds of raw materials quality are than being 1:1.5:1.
A, B component material are reacted after pressing the mixing of A:B=100:100 weight proportion, can obtain inorganic modified mine polyurethane reinforcement material, its product quality indicator is as follows:
Embodiment 3
100 kilograms, preparation component A material, weigh respectively: polyether glycol 50 kilograms, polyester polyol 8 kilograms, inorganic modifier A 8 kilograms, inorganic modifier B 2 kilograms, suds-stabilizing agent AK-88721 kilogram, the chloro-1-fluoroethane of whipping agent 1,1-bis-7 kilograms, solubilizing agent OP-101.7 kilogram, catalyst dibutyltin dilaurylate 0.65 kilogram, catalyzer 2,4,6-tri-(dimethylamino methyl) phenol 1.35 kilograms, catalyzer five methyl diethylentriamine 0.6 kilogram, fire retardant trichloropropyl phosphate 19.7 kilograms.Load weighted polyether glycol and polyester polyol are loaded in mixing kettle and stirs, then add the inorganic modifier A weighed up respectively, inorganic modifier B, suds-stabilizing agent, whipping agent, solubilizing agent, catalyzer, fire retardant stirs at normal temperatures, after sampling detection is qualified, gets final product barrelling.
100 kilograms, preparation B component material, weighs: poly methylene poly phenyl poly isocyanate 65 kilograms, '-diphenylmethane diisocyanate 10 kilograms, composite modifier 25 kilograms respectively.
Wherein:
Polyether glycol adopts functionality to be 8, and molecular weight is the poly(propylene oxide) ethoxylated polyhydric alcohol of 1000,
Polyester polyol adopts functionality to be 2, and molecular weight is the benzoic anhydride polyester polyol of 1000,
Inorganic modifier A employing degree Beaume is the potassium silicate aqueous solution of 60 degree,
Inorganic modifier B is a kind of median size be mixed by calcium carbonate, barium sulfate, kaolin and trimeric cyanamide is the superfine powder of 30um, and four kinds of raw materials quality ratios are 1:1.5:2:1,
Composite modifier is mixed by dimethyl phthalate, dibutyl phthalate and dioctyl phthalate (DOP), and three kinds of raw materials quality are than being 1:2:1.5.
A, B component material are reacted after pressing the mixing of A:B=100:100 weight proportion, can obtain inorganic modified mine polyurethane reinforcement material, its product quality indicator is as follows:
。
Claims (10)
1. an inorganic modified mine polyurethane reinforcement material, is polymerized by component A and B component, it is characterized in that:
The raw material of component A, is calculated in mass percent, and proportioning is as follows:
The raw material of B component, is calculated in mass percent, and proportioning is as follows:
Poly methylene poly phenyl poly isocyanate: 50 ~ 75%
'-diphenylmethane diisocyanate: 10 ~ 20%
Composite modifier: 10 ~ 30%.
2. inorganic modified mine polyurethane reinforcement material according to claim 1, is characterized in that: the weight ratio of A, B component is A:B=1:1.
3. inorganic modified mine polyurethane reinforcement material according to claim 1, is characterized in that: polyether glycol adopts functionality to be 8, and molecular weight is the poly(propylene oxide) ethoxylated polyhydric alcohol of 300 ~ 1000; Polyester polyol adopts functionality to be 2, and molecular weight is the benzoic anhydride polyester polyol of 400 ~ 1000.
4. inorganic modified mine polyurethane reinforcement material according to claim 1, is characterized in that: inorganic modifier A employing degree Beaume is the potassium silicate aqueous solution of 20 ~ 60 degree.
5. inorganic modified mine polyurethane reinforcement material according to claim 1, it is characterized in that: inorganic modifier B is the superfine powder that a kind of median size be mixed by calcium carbonate, barium sulfate, kaolin and trimeric cyanamide is less than 50 μm, four kinds of raw materials quality are than being 1:1.5:2:1.
6. inorganic modified mine polyurethane reinforcement material according to claim 1, is characterized in that: suds-stabilizing agent adopts Si-C class tensio-active agent, and whipping agent adopts the chloro-1-fluoroethane of 1,1-bis-.
7. inorganic modified mine polyurethane reinforcement material according to claim 1, is characterized in that: solubilizing agent is alkylphenol-polyethenoxy base ether nonionic type tensio-active agent, adopts OP-10; Fire retardant is phosphate ester flame retardants, adopts trichloropropyl phosphate.
8. inorganic modified mine polyurethane reinforcement material according to claim 1, it is characterized in that: catalyzer is organo-metallic catalyst and organic amine catalyst, adopt dibutyl tin laurate, 2,4,6-tri-(dimethylamino methyl) phenol and five methyl diethylentriamine, the mass ratio between three is 0.5 ~ 1.5:1 ~ 2.5:0.5 ~ 2.
9. inorganic modified mine polyurethane reinforcement material according to claim 1, it is characterized in that: composite modifier is mixed by dimethyl phthalate, dibutyl phthalate and dioctyl phthalate (DOP), three kinds of raw materials quality are than being 1:0-2:1-1.5.
10. a preparation method for the arbitrary described inorganic modified mine polyurethane reinforcement material of claim 1-9, is characterized in that: comprise the following steps:
(1) component A material is prepared: first stir in load weighted polyether glycol, polyester polyol loading mixing kettle, then load weighted inorganic modifier A, inorganic modifier B, catalyzer, whipping agent, solubilizing agent, suds-stabilizing agent, fire retardant is added, even in stirring at normal temperature, get final product barrelling;
(2) B component material is prepared: stir in load weighted poly methylene poly phenyl poly isocyanate, '-diphenylmethane diisocyanate, composite modifier loading mixing kettle, get final product barrelling;
(3) A, B component material are mixed by the weight ratio of A:B=1:1, obtain inorganic modified mine polyurethane reinforcement material.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104830052A (en) * | 2015-05-21 | 2015-08-12 | 淄博润义金环保新材料科技有限公司 | Modified polyurethane filling material for tunnel and preparation method thereof |
| CN104927021A (en) * | 2015-05-21 | 2015-09-23 | 淄博润义金环保新材料科技有限公司 | Polyurethane material for tunnel water plugging and preparation method thereof |
| CN105001397A (en) * | 2015-05-21 | 2015-10-28 | 淄博润义金环保新材料科技有限公司 | Tunnel strengthening polyurethane material and preparation method thereof |
| CN106750160A (en) * | 2016-12-02 | 2017-05-31 | 上海东大聚氨酯有限公司 | A kind of highway reparation polyurethane raw material composition and its application method |
| CN107417876A (en) * | 2017-06-13 | 2017-12-01 | 山东润义金新材料科技股份有限公司 | Colliery macromolecule slip casting strengthening material and preparation method thereof |
| CN109306072A (en) * | 2018-09-30 | 2019-02-05 | 山东诺威新材料有限公司 | Frozen soil polyurethane reinforcement material and preparation method thereof |
| CN110204729A (en) * | 2019-07-15 | 2019-09-06 | 上海麦浦新材料科技有限公司 | A kind of silicone copolymer surfactants and its purposes in liquefied natural gas heat preservation rigid foam |
| CN111057365A (en) * | 2019-12-31 | 2020-04-24 | 北京中矿恒安科技有限公司 | Low-temperature organic reinforcing material and preparation method thereof |
| CN112778483A (en) * | 2020-12-30 | 2021-05-11 | 山东一诺威新材料有限公司 | Low-temperature type bi-component polyurethane material for coal rock mass reinforcement field and preparation method thereof |
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