CN103304771B - Polyurethane reinforced material and preparation method thereof - Google Patents
Polyurethane reinforced material and preparation method thereof Download PDFInfo
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- CN103304771B CN103304771B CN201310237776.0A CN201310237776A CN103304771B CN 103304771 B CN103304771 B CN 103304771B CN 201310237776 A CN201310237776 A CN 201310237776A CN 103304771 B CN103304771 B CN 103304771B
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Abstract
The invention discloses a polyurethane reinforced material which is characterized by comprising a component A and a component B, wherein the component A comprises the following components in parts by weight: 20-45 parts of polyether polyol A, 25-55 parts of polyether polyol B, 5-10 parts of polyether polyol C, 5-15 parts of a flame retardant A, 5-10 parts of a flame retardant B, 0.2-0.5 parts of an amine catalyst, 0.1-0.5 parts of a tin catalyst and 0.5-1.0 parts of a foam stabilizer, and the component B is polymethylene polyphenyl polyisocyanate. The polyurethane reinforced material further comprises 3-8 parts of a viscosity reducer. Compared with similar materials, the material has better permeability and higher mechanical property, and broken coal and rock masses can be fixedly combined integrally and effectively due to ultrahigh tensile compressive strength and binding performance, so that the top plate and two uppers can bear pressure actively. The material does not contain poisonous volatile and corrosive matters, so that the material satisfies the demand of safety and environment-friendliness of materials under the shaft.
Description
Technical field
The invention belongs to technical field of polymer materials, particularly relate to a kind of high strength fractured roof and control urethane reinforcement material and preparation method thereof.
Background technology
Coal mine roof plate disaster is one of accident that in coal mining accident, lethal number is maximum, all the time for the important process of the improvement Dou Shi coal mining enterprise of roof fall accident.Polyurethanes reinforcement material has good consolidation to fractured coal and rock, is nowadays that the roof accident that colliery is most widely used administers material.And continuing to increase along with the colliery depth of excavation, the pressure that top board bears is also increasing, especially along with the increase of rock burst occurrence frequency, to the shock resistance of top board and the requirement of anti-pressure ability more and more higher, conventional polyurethanes reinforcement material adds intrinsic good effect for the coal and rock under usual terms, but be difficult to meet the demands under above-mentioned special conditions, therefore need the higher material of a kind of intensity to solve problems.
Summary of the invention
For the deficiencies in the prior art, the object of this invention is to provide a kind of urethane reinforcement material, this material has very high ultimate compression strength, tensile strength and cohesive strength.
Another object of the present invention is to provide a kind of preparation method of above-mentioned urethane reinforcement material, and the method is simple.
To achieve these goals, technical scheme of the present invention is as follows:
The invention provides a kind of urethane reinforcement material, comprise component A and B component,
Described component A comprises the component of following weight part:
Polyether glycol A is 20 ~ 45 parts, and polyether glycol B is 25 ~ 55 parts, and polyether glycol C is 5 ~ 10 parts, fire retardant A is 5 ~ 15 parts, and fire retardant B is 5 ~ 10 parts, and amines catalyst is 0.2 ~ 0.5 part, tin class catalyzer is 0.1 ~ 0.5 part, and suds-stabilizing agent is 0.5 ~ 1.0 part;
Described B component is poly methylene poly phenyl poly isocyanate.
As the preferred technical scheme of one, described urethane reinforcement material also comprises viscosity-depression agent 3 ~ 8 parts.
As the preferred technical scheme of one, described viscosity-depression agent is diethylene glycol monoethyl ether.
As the preferred technical scheme of one, the functionality of described polyether glycol A is 2 ~ 4, and molecular weight is 800 ~ 1200, and viscosity is 400 ~ 1000mPa.s.
As the preferred technical scheme of one, the functionality of described polyether glycol B is 2 ~ 4, and molecular weight is 500 ~ 800, and viscosity is 300 ~ 600mPa.s.
As the preferred technical scheme of one, the functionality of described polyether glycol C is 3 ~ 5, and molecular weight is 200 ~ 400, and viscosity is 1000 ~ 1500mPa.s.
As the preferred technical scheme of one, described fire retardant A is dimethyl methyl phosphonate.
As the preferred technical scheme of one, described fire retardant B is three (2-chloroethyl) phosphoric acid ester or three (2-chloropropyl) phosphoric acid ester.
As the preferred technical scheme of one, described tin class catalyzer is dibutyl tin laurate.
As the preferred technical scheme of one, described amines catalyst is gel-like catalyzer or foaming kind catalyzer.
As the preferred technical scheme of one, described gel-like catalyzer is dimethylcyclohexylamine.
As the preferred technical scheme of one, described foaming kind catalyzer is five methyl diethylentriamine.
As the preferred technical scheme of one, described suds-stabilizing agent is silicone oil suds-stabilizing agent, uses the trade mark to be AK-8803, AK-8805 or H-3612.
As the preferred technical scheme of one, described poly methylene poly phenyl poly isocyanate is brown transparent liquid, and viscosity is 150 ~ 250mPa.s ,-NCO (wt%) is 30.5 ~ 32%.
As the preferred technical scheme of one, the volume ratio of described component A and B component is 1:1 or mass ratio is 1:1.17.
Present invention also offers a kind of preparation method of above-mentioned urethane reinforcement material, comprise the following steps:
The preparation method of described component A is as follows:
Be 20 ~ 45 parts by polyether glycol A, polyether glycol B is 25 ~ 55 parts, polyether glycol C is 5 ~ 10 parts of mixing, to add fire retardant A be 5 ~ 15 parts and fire retardant B is 5 ~ 10 parts of mixing, finally add that amines catalyst is 0.2 ~ 0.5 part, tin class catalyzer is that 0.1 ~ 0.5 part and suds-stabilizing agent are 0.5 ~ 1.0 part and stir, prepare component A;
Component A and the B component of to be 1:1 or mass ratio by volume ratio be 1:1.17 mix, solidify, and obtain urethane reinforcement material.
Present invention also offers a kind of preparation method of above-mentioned urethane reinforcement material, comprise the following steps:
The preparation method of described component A is as follows:
Be 20 ~ 45 parts by polyether glycol A, polyether glycol B is 25 ~ 55 parts, polyether glycol C is 5 ~ 10 parts of mixing, to add fire retardant A be 5 ~ 15 parts and fire retardant B is 5 ~ 10 parts of mixing, finally add that amines catalyst is 0.2 ~ 0.5 part, tin class catalyzer is 0.1 ~ 0.5 part, suds-stabilizing agent is that 0.5 ~ 1.0 part and viscosity-depression agent are 3 ~ 8 parts and stir, prepare component A;
Component A and the B component of to be 1:1 or mass ratio by volume ratio be 1:1.17 mix, solidify, and obtain urethane reinforcement material.
The present invention compared with prior art, has the following advantages and beneficial effect:
1, in material of the present invention, component A, B component all have very low viscosity, and perviousness is fine, can penetrate in extremely trickle coal and rock crack.
2, material cured speed of the present invention can carry out condition according to requirement of engineering, large between regulatory region.
3, material mechanical performance of the present invention is very superior, is specially adapted to the fractured roof that pressure-bearing is larger.
4, materials application adaptability of the present invention is good, and component A, B component are suitable for the situation that certain deviation occurs proportioning, and product still has higher mechanical property.
5, material of the present invention is mainly used in the field of reinforcement solving colliery fractured roof, is particularly useful for the reinforcing of the Deep Mine fractured roof having larger pressure-bearing, can the generation of effectively controlroof inbreak and side falling accident.
6, material preparation method of the present invention is simple, by can prepare the reinforcement material of excellent property to raw-material mixtures such as polyvalent alcohol, fire retardant, catalyzer, suds-stabilizing agent, viscosity-depression agent and isocyanic ester, material is injected in coal and rock by Double-liquid mud-injection pump, can reach the function of reinforcing coal rock mass after fast setting.
7, material of the present invention has the mechanical property of better perviousness and Geng Gao compared with material of the same type, and the compression and tensile strength of superelevation and adhesive property can, effectively as a whole for fractured coal and rock consolidation, make top board and two help energy initiatively pressure-bearing; Material containing toxic volatile and corrosives, does not meet down-hole to the safety of material and environmental requirement; Material greatly can improve the supporting capacity of top board after using, and can resist and certain press impact, can meet the reinforcement criteria of deep-well tunnel preferably.
Embodiment
Below in conjunction with embodiment, the present invention is further detailed explanation.
Poly methylene poly phenyl poly isocyanate used is below brown transparent liquid, and viscosity is 150 ~ 250mPa.s ,-NCO (wt%) is 30.5 ~ 32%.
Material properties test of the present invention is tested according to method described in " colliery reinforcing coal rock mass macromolecular material " industry standard.
Set time: component A, B component by volume 1:1 weigh required quality (converting according to tested density), and A+B total mass is no less than 200g, and after stirring with glass stick, recording materials are from being mixed into the immobilising time.
Viscosity: the kinetic viscosity using rotor rotational viscosimeter test liquid material.
Ultimate compression strength is tested according to " GB/T2567-2008 resin-cast body method for testing performance ".
Tensile strength is tested according to " GB/T2567-2008 resin-cast body method for testing performance ".
Slip resistance is tested according to " GB/T10007-2008 rigid foam shear strength test method ".
Cohesive strength is tested according to " GB/T7124-2008 tackiness agent draws high the mensuration (rigid material is to rigid material) of shearing resistance ".
Flame retardant resistance is according to MT113-1995 standard testing.
Embodiment 1
Preparation component A 50kg: weighing polyether glycol A(functionality is 2 ~ 4, molecular weight is 800 ~ 1200, viscosity is 400 ~ 1000mPa.s) 33 parts, how far alcohol B(functionality is 2 ~ 4 to polyethers, molecular weight is 500 ~ 800, viscosity is 300 ~ 600mPa.s) 35 parts, polyether glycol C(functionality is 3 ~ 5, molecular weight is 200 ~ 400, viscosity is 1000 ~ 1500mPa.s) 6 parts, dimethyl methyl phosphonate 10 parts, three (2-chloroethyl) phosphoric acid ester 8 parts, dibutyl tin laurate 0.3 part, dimethylcyclohexylamine 0.2 part, five methyl diethylentriamine 0.2 part, silicone oil suds-stabilizing agent AK-8805 is 0.5 part, diethylene glycol monoethyl ether 6.8 parts, load in the small-sized mixing kettle of 100L, after stirring under normal temperature and pressure, barrelling sealing is for subsequent use.
B component is poly methylene poly phenyl poly isocyanate.
By the proportional sampling of component A, B component 1:1 or 1:1.17 in mass ratio by volume, application apparatus is pneumatic Double-liquid mud-injection pump and corollary apparatus thereof; Total mass needed for test request calculates required each constituent mass, sufficient for mixing material is poured into self-vulcanizing in Standard Module, tests mechanical index after cooling.Adhesive property presses the strict sample preparation of standard-required, puts into 25 DEG C of baking ovens and preserves test after at least 3 hours.
The performance that preparation-obtained high strength fractured roof controls urethane reinforcement material is as follows:
Set time (25 DEG C): 80 seconds
Viscosity (25 DEG C): 286mPa.s
Ultimate compression strength: 75.4MPa
Tensile strength: 34.6MPa
Shear strength: 22.1MPa
Cohesive strength: 6.3MPa
Flame retardant resistance: spirit lamp experiment flaming combustion 2.3 seconds.
Embodiment 2
Preparation component A 50kg: weighing polyether glycol A(functionality is 2 ~ 4, molecular weight is 800 ~ 1200, viscosity is 400 ~ 1000mPa.s) 28 parts, how far alcohol B(functionality is 2 ~ 4 to polyethers, molecular weight is 500 ~ 800, viscosity is 300 ~ 600mPa.s) 40 parts, polyether glycol C(functionality is 3 ~ 5, molecular weight is 200 ~ 400, viscosity is 1000 ~ 1500mPa.s) 8 parts, dimethyl methyl phosphonate 13 parts, three (2-chloropropyl) phosphoric acid ester 5 parts, dibutyl tin laurate 0.2 part, dimethylcyclohexylamine 0.3 part, five methyl diethylentriamine 0.2 part, silicone oil suds-stabilizing agent H-3612 is 0.5 part, diethylene glycol monoethyl ether 4.8 parts, load in the small-sized mixing kettle of 100L, after stirring under normal temperature and pressure, barrelling sealing is for subsequent use.
B component is poly methylene poly phenyl poly isocyanate.
By the proportional sampling of component A, B component 1:1 or 1:1.17 in mass ratio by volume, application apparatus is pneumatic Double-liquid mud-injection pump and corollary apparatus thereof; Total mass needed for test request calculates required each constituent mass, sufficient for mixing material is poured into self-vulcanizing in Standard Module, tests mechanical index after cooling.Adhesive property presses the strict sample preparation of standard-required, puts into 25 DEG C of baking ovens and preserves test after at least 3 hours.
The performance that preparation-obtained high strength fractured roof controls urethane reinforcement material is as follows:
Set time (25 DEG C): 78 seconds
Viscosity (25 DEG C): 248mPa.s
Ultimate compression strength: 83.5MPa
Tensile strength: 38.6MPa
Shear strength: 25.7MPa
Cohesive strength: 6.7MPa
Flame retardant resistance: spirit lamp experiment flaming combustion 2.4 seconds.
Embodiment 3
Preparation component A 50kg: weighing polyether glycol A(functionality is 2 ~ 4, molecular weight is 800 ~ 1200, viscosity is 400 ~ 1000mPa.s) 20 parts, how far alcohol B(functionality is 2 ~ 4 to polyethers, molecular weight is 500 ~ 800, viscosity is 300 ~ 600mPa.s) 48 parts, polyether glycol C(functionality is 3 ~ 5, molecular weight is 200 ~ 400, viscosity is 1000 ~ 1500mPa.s) 9 parts, dimethyl methyl phosphonate 8 parts, three (2-chloroethyl) phosphoric acid ester 3 parts, three (2-chloropropyl) phosphoric acid ester 7 parts, dibutyl tin laurate 0.45 part, five methyl diethylentriamine 0.25 part, silicone oil suds-stabilizing agent H-3612 is 0.5 part, diethylene glycol monoethyl ether 3.8 parts, load in the small-sized mixing kettle of 100L, after stirring under normal temperature and pressure, barrelling sealing is for subsequent use.
B component is poly methylene poly phenyl poly isocyanate.
By the proportional sampling of component A, B component 1:1 or 1:1.17 in mass ratio by volume, application apparatus is pneumatic Double-liquid mud-injection pump and corollary apparatus thereof; Total mass needed for test request calculates required each constituent mass, sufficient for mixing material is poured into self-vulcanizing in Standard Module, tests mechanical index after cooling.Adhesive property presses the strict sample preparation of standard-required, puts into 25 DEG C of baking ovens and preserves test after at least 3 hours.
The performance that preparation-obtained high strength fractured roof controls urethane reinforcement material is as follows:
Set time (25 DEG C): 76 seconds
Viscosity (25 DEG C): 192mPa.s
Ultimate compression strength: 91.8MPa
Tensile strength: 43.2MPa
Shear strength: 29.1MPa
Cohesive strength: 7.4MPa
Flame retardant resistance: spirit lamp experiment flaming combustion 2.8 seconds.
As can be seen from above embodiment 1 ~ 3, material mechanical performance of the present invention is far away higher than the requirement of industry standard, and mechanical index can reach:
Ultimate compression strength: >=60MPa
Tensile strength: >=30MPa
Slip resistance: >=20MPa
Cohesive strength: >=6MPa
Flame retardant resistance: meet MT113-1995 requirement.
Embodiment 4
The preparation method of component A is as follows:
Be 2 ~ 4 by polyether glycol A(functionality, molecular weight is 800 ~ 1200, viscosity is 400 ~ 1000mPa.s) be 20 parts, polyether glycol B(functionality is 2 ~ 4, molecular weight is 500 ~ 800, viscosity is 300 ~ 600mPa.s) be 55 parts, polyether glycol C(functionality is 3 ~ 5, molecular weight is 200 ~ 400, viscosity is 1000 ~ 1500mPa.s) be 5 parts of mixing, to add fire retardant A dimethyl methyl phosphonate be 12 parts and fire retardant B tri-(2-chloroethyl) phosphoric acid ester is 7 parts of mixing, finally add amines catalyst dimethylcyclohexylamine 0.2 part, tin class catalyst dibutyltin dilaurylate 0.1 part and silicone oil suds-stabilizing agent AK-8803 are 0.7 part and stir, prepare component A,
B component is poly methylene poly phenyl poly isocyanate.
By the proportional sampling of component A, B component 1:1 or 1:1.17 in mass ratio by volume, application apparatus is pneumatic Double-liquid mud-injection pump and corollary apparatus thereof; Total mass needed for test request calculates required each constituent mass, sufficient for mixing material is poured into self-vulcanizing in Standard Module, tests mechanical index after cooling.Adhesive property presses the strict sample preparation of standard-required, puts into 25 DEG C of baking ovens and preserves test after at least 3 hours.
Set time (25 DEG C): 93 seconds
Viscosity (25 DEG C): 278mPa.s
Ultimate compression strength: 85.4MPa
Tensile strength: 37.2MPa
Shear strength: 22.6MPa
Cohesive strength: 7.1MPa
Flame retardant resistance: spirit lamp experiment flaming combustion 1.8 seconds.
Embodiment 5
The preparation method of component A is as follows:
Be 2 ~ 4 by polyether glycol A(functionality, molecular weight is 800 ~ 1200, viscosity is 400 ~ 1000mPa.s) be 45 parts, polyether glycol B(functionality is 2 ~ 4, molecular weight is 500 ~ 800, viscosity is 300 ~ 600mPa.s) be 25 parts, polyether glycol C(functionality is 3 ~ 5, molecular weight is 200 ~ 400, viscosity is 1000 ~ 1500mPa.s) be 10 parts of mixing, to add fire retardant A dimethyl methyl phosphonate be 9 parts and fire retardant B tri-(2-chloroethyl) phosphoric acid ester is 9 parts of mixing, finally add amines catalyst dimethylcyclohexylamine 0.5 part, tin class catalyst dibutyltin dilaurylate 0.5 part and silicone oil suds-stabilizing agent AK-8803 are 1.0 parts and stir, prepare component A,
B component is poly methylene poly phenyl poly isocyanate.
By the proportional sampling of component A, B component 1:1 or 1:1.17 in mass ratio by volume, application apparatus is pneumatic Double-liquid mud-injection pump and corollary apparatus thereof; Total mass needed for test request calculates required each constituent mass, sufficient for mixing material is poured into self-vulcanizing in Standard Module, tests mechanical index after cooling.Adhesive property presses the strict sample preparation of standard-required, puts into 25 DEG C of baking ovens and preserves test after at least 3 hours.
Set time (25 DEG C): 52 seconds
Viscosity (25 DEG C): 302mPa.s
Ultimate compression strength: 81.2MPa
Tensile strength: 35.4MPa
Shear strength: 21.3MPa
Cohesive strength: 7.5MPa
Flame retardant resistance: spirit lamp experiment flaming combustion 2.8 seconds.
Embodiment 6
The preparation method of component A is as follows:
Be 2 ~ 4 by polyether glycol A(functionality, molecular weight is 800 ~ 1200, viscosity is 400 ~ 1000mPa.s) be 25 parts, polyether glycol B(functionality is 2 ~ 4, molecular weight is 500 ~ 800, viscosity is 300 ~ 600mPa.s) be 50 parts, polyether glycol C(functionality is 3 ~ 5, molecular weight is 200 ~ 400, viscosity is 1000 ~ 1500mPa.s) be 10 parts of mixing, to add fire retardant A dimethyl methyl phosphonate be 5 parts and fire retardant B tri-(2-chloroethyl) phosphoric acid ester is 8 parts of mixing, finally add amines catalyst dimethylcyclohexylamine 0.5 part, tin class catalyst dibutyltin dilaurylate 0.5 part and silicone oil suds-stabilizing agent AK-8803 are 1.0 parts and stir, prepare component A,
B component is poly methylene poly phenyl poly isocyanate.
By the proportional sampling of component A, B component 1:1 or 1:1.17 in mass ratio by volume, application apparatus is pneumatic Double-liquid mud-injection pump and corollary apparatus thereof; Total mass needed for test request calculates required each constituent mass, sufficient for mixing material is poured into self-vulcanizing in Standard Module, tests mechanical index after cooling.Adhesive property presses the strict sample preparation of standard-required, puts into 25 DEG C of baking ovens and preserves test after at least 3 hours.
Set time (25 DEG C): 48 seconds
Viscosity (25 DEG C): 325mPa.s
Ultimate compression strength: 98.7MPa
Tensile strength: 47.6MPa
Shear strength: 32.5MPa
Cohesive strength: 7.8MPa
Flame retardant resistance: spirit lamp experiment flaming combustion 3.8 seconds (not meeting standard-required).
Embodiment 7
The preparation method of component A is as follows:
Be 2 ~ 4 by polyether glycol A(functionality, molecular weight is 800 ~ 1200, viscosity is 400 ~ 1000mPa.s) be 35 parts, polyether glycol B(functionality is 2 ~ 4, molecular weight is 500 ~ 800, viscosity is 300 ~ 600mPa.s) be 30 parts, polyether glycol C(functionality is 3 ~ 5, molecular weight is 200 ~ 400, viscosity is 1000 ~ 1500mPa.s) be 9 parts of mixing, to add fire retardant A dimethyl methyl phosphonate be 15 parts and fire retardant B tri-(2-chloroethyl) phosphoric acid ester is 10 parts of mixing, finally add amines catalyst dimethylcyclohexylamine 0.3 part, tin class catalyst dibutyltin dilaurylate 0.1 part and silicone oil suds-stabilizing agent AK-8803 are 0.6 part and stir, prepare component A,
B component is poly methylene poly phenyl poly isocyanate.
By the proportional sampling of component A, B component 1:1 or 1:1.17 in mass ratio by volume, application apparatus is pneumatic Double-liquid mud-injection pump and corollary apparatus thereof; Total mass needed for test request calculates required each constituent mass, sufficient for mixing material is poured into self-vulcanizing in Standard Module, tests mechanical index after cooling.Adhesive property presses the strict sample preparation of standard-required, puts into 25 DEG C of baking ovens and preserves test after at least 3 hours.
Set time (25 DEG C): 95 seconds
Viscosity (25 DEG C): 263mPa.s
Ultimate compression strength: 80.2MPa
Tensile strength: 36.3MPa
Shear strength: 25.6MPa
Cohesive strength: 6.8MPa
Flame retardant resistance: spirit lamp experiment flaming combustion 1.5 seconds.
Embodiment 8
The preparation method of component A is as follows:
Be 2 ~ 4 by polyether glycol A(functionality, molecular weight is 800 ~ 1200, viscosity is 400 ~ 1000mPa.s) be 33 parts, polyether glycol B(functionality is 2 ~ 4, molecular weight is 500 ~ 800, viscosity is 300 ~ 600mPa.s) be 35 parts, polyether glycol C(functionality is 3 ~ 5, molecular weight is 200 ~ 400, viscosity is 1000 ~ 1500mPa.s) be 6 parts of mixing, to add fire retardant A dimethyl methyl phosphonate be 10 parts and fire retardant B tri-(2-chloroethyl) phosphoric acid ester is 8 parts of mixing, diethylene glycol monoethyl ether 6.8 parts, finally add amines catalyst dimethylcyclohexylamine 0.4 part, tin class catalyst dibutyltin dilaurylate 0.3 part and silicone oil suds-stabilizing agent AK-8803 are 0.5 part and stir, prepare component A,
B component is poly methylene poly phenyl poly isocyanate.
By the proportional sampling of component A, B component 1:1 or 1:1.17 in mass ratio by volume, application apparatus is pneumatic Double-liquid mud-injection pump and corollary apparatus thereof; Total mass needed for test request calculates required each constituent mass, sufficient for mixing material is poured into self-vulcanizing in Standard Module, tests mechanical index after cooling.Adhesive property presses the strict sample preparation of standard-required, puts into 25 DEG C of baking ovens and preserves test after at least 3 hours.
Set time (25 DEG C): 82 seconds
Viscosity (25 DEG C): 289mPa.s
Ultimate compression strength: 76.8MPa
Tensile strength: 35.2MPa
Shear strength: 22.9MPa
Cohesive strength: 6.5MPa
Flame retardant resistance: spirit lamp experiment flaming combustion 2.5 seconds.
Embodiment 9
The preparation method of component A is as follows:
Be 2 ~ 4 by polyether glycol A(functionality, molecular weight is 800 ~ 1200, viscosity is 400 ~ 1000mPa.s) be 28 parts, polyether glycol B(functionality is 2 ~ 4, molecular weight is 500 ~ 800, viscosity is 300 ~ 600mPa.s) be 40 parts, polyether glycol C(functionality is 3 ~ 5, molecular weight is 200 ~ 400, viscosity is 1000 ~ 1500mPa.s) be 8 parts of mixing, to add fire retardant A dimethyl methyl phosphonate be 13 parts and fire retardant B tri-(2-chloroethyl) phosphoric acid ester is 5 parts of mixing, diethylene glycol monoethyl ether 4.8 parts, finally add amines catalyst dimethylcyclohexylamine 0.5 part, tin class catalyst dibutyltin dilaurylate 0.2 part and silicone oil suds-stabilizing agent AK-8803 are 0.5 part and stir, prepare component A,
B component is poly methylene poly phenyl poly isocyanate.
By the proportional sampling of component A, B component 1:1 or 1:1.17 in mass ratio by volume, application apparatus is pneumatic Double-liquid mud-injection pump and corollary apparatus thereof; Total mass needed for test request calculates required each constituent mass, sufficient for mixing material is poured into self-vulcanizing in Standard Module, tests mechanical index after cooling.Adhesive property presses the strict sample preparation of standard-required, puts into 25 DEG C of baking ovens and preserves test after at least 3 hours.
Set time (25 DEG C): 88 seconds
Viscosity (25 DEG C): 271mPa.s
Ultimate compression strength: 81.6MPa
Tensile strength: 36.8MPa
Shear strength: 23.5MPa
Cohesive strength: 6.4MPa
Flame retardant resistance: spirit lamp experiment flaming combustion 2.8 seconds.
Embodiment 10
The preparation method of component A is as follows:
Be 2 ~ 4 by polyether glycol A(functionality, molecular weight is 800 ~ 1200, viscosity is 400 ~ 1000mPa.s) be 20 parts, polyether glycol B(functionality is 2 ~ 4, molecular weight is 500 ~ 800, viscosity is 300 ~ 600mPa.s) be 48 parts, polyether glycol C(functionality is 3 ~ 5, molecular weight is 200 ~ 400, viscosity is 1000 ~ 1500mPa.s) be 9 parts of mixing, to add fire retardant A dimethyl methyl phosphonate be 8 parts and fire retardant B tri-(2-chloropropyl) phosphoric acid ester is 10 parts of mixing, diethylene glycol monoethyl ether 3.8 parts, finally add amines catalyst five methyl diethylentriamine 0.25 part, tin class catalyst dibutyltin dilaurylate 0.45 part and silicone oil suds-stabilizing agent H-3612 are 0.5 part and stir, prepare component A,
B component is poly methylene poly phenyl poly isocyanate.
By the proportional sampling of component A, B component 1:1 or 1:1.17 in mass ratio by volume, application apparatus is pneumatic Double-liquid mud-injection pump and corollary apparatus thereof; Total mass needed for test request calculates required each constituent mass, sufficient for mixing material is poured into self-vulcanizing in Standard Module, tests mechanical index after cooling.Adhesive property presses the strict sample preparation of standard-required, puts into 25 DEG C of baking ovens and preserves test after at least 3 hours.
Set time (25 DEG C): 78 seconds
Viscosity (25 DEG C): 305mPa.s
Ultimate compression strength: 90.6MPa
Tensile strength: 44.8MPa
Shear strength: 29.7MPa
Cohesive strength: 7.3MPa
Flame retardant resistance: spirit lamp experiment flaming combustion 2.5 seconds.
Embodiment 11
The preparation method of component A is as follows:
Be 2 ~ 4 by polyether glycol A(functionality, molecular weight is 800 ~ 1200, viscosity is 400 ~ 1000mPa.s) be 35 parts, polyether glycol B(functionality is 2 ~ 4, molecular weight is 500 ~ 800, viscosity is 300 ~ 600mPa.s) be 44 parts, polyether glycol C(functionality is 3 ~ 5, molecular weight is 200 ~ 400, viscosity is 1000 ~ 1500mPa.s) be 5 parts of mixing, to add fire retardant A dimethyl methyl phosphonate be 6 parts and fire retardant B tri-(2-chloroethyl) phosphoric acid ester is 9 parts of mixing, finally add amines catalyst dimethylcyclohexylamine 0.35 part, tin class catalyst dibutyltin dilaurylate 0.15 part and silicone oil suds-stabilizing agent AK-8805 are 0.5 part and stir, prepare component A,
B component is poly methylene poly phenyl poly isocyanate.
By the proportional sampling of component A, B component 1:1 or 1:1.17 in mass ratio by volume, application apparatus is pneumatic Double-liquid mud-injection pump and corollary apparatus thereof; Total mass needed for test request calculates required each constituent mass, sufficient for mixing material is poured into self-vulcanizing in Standard Module, tests mechanical index after cooling.Adhesive property presses the strict sample preparation of standard-required, puts into 25 DEG C of baking ovens and preserves test after at least 3 hours.
Set time (25 DEG C): 86 seconds
Viscosity (25 DEG C): 312mPa.s
Ultimate compression strength: 78.6MPa
Tensile strength: 35.2MPa
Shear strength: 22.3MPa
Cohesive strength: 6.8MPa
Flame retardant resistance: spirit lamp experiment flaming combustion 2.8 seconds.
Embodiment 12
The preparation method of component A is as follows:
Be 2 ~ 4 by polyether glycol A(functionality, molecular weight is 800 ~ 1200, viscosity is 400 ~ 1000mPa.s) be 43 parts, polyether glycol B(functionality is 2 ~ 4, molecular weight is 500 ~ 800, viscosity is 300 ~ 600mPa.s) be 28 parts, polyether glycol C(functionality is 3 ~ 5, molecular weight is 200 ~ 400, viscosity is 1000 ~ 1500mPa.s) be 10 parts of mixing, to add fire retardant A dimethyl methyl phosphonate be 5 parts and fire retardant B tri-(2-chloroethyl) phosphoric acid ester is 10.1 parts of mixing, finally add amines catalyst dimethylcyclohexylamine 0.2 part, tin class catalyst dibutyltin dilaurylate 0.1 part, silicone oil suds-stabilizing agent AK-8805 is 0.6 part and stirs with viscosity-depression agent diethylene glycol monoethyl ether 3 parts, prepare component A,
B component is poly methylene poly phenyl poly isocyanate.
By the proportional sampling of component A, B component 1:1 or 1:1.17 in mass ratio by volume, application apparatus is pneumatic Double-liquid mud-injection pump and corollary apparatus thereof; Total mass needed for test request calculates required each constituent mass, sufficient for mixing material is poured into self-vulcanizing in Standard Module, tests mechanical index after cooling.Adhesive property presses the strict sample preparation of standard-required, puts into 25 DEG C of baking ovens and preserves test after at least 3 hours.
Set time (25 DEG C): 95 seconds
Viscosity (25 DEG C): 248mPa.s
Ultimate compression strength: 83.6MPa
Tensile strength: 37.2MPa
Shear strength: 23.5MPa
Cohesive strength: 7.0MPa
Flame retardant resistance: spirit lamp experiment flaming combustion 3.0 seconds.
Embodiment 13
The preparation method of component A is as follows:
Be 2 ~ 4 by polyether glycol A(functionality, molecular weight is 800 ~ 1200, viscosity is 400 ~ 1000mPa.s) be 24 parts, polyether glycol B(functionality is 2 ~ 4, molecular weight is 500 ~ 800, viscosity is 300 ~ 600mPa.s) be 37 parts, polyether glycol C(functionality is 3 ~ 5, molecular weight is 200 ~ 400, viscosity is 1000 ~ 1500mPa.s) be 5 parts of mixing, to add fire retardant A dimethyl methyl phosphonate be 15 parts and fire retardant B tri-(2-chloroethyl) phosphoric acid ester is 9.5 parts of mixing, finally add amines catalyst dimethylcyclohexylamine 0.3 part, tin class catalyst dibutyltin dilaurylate 0.4 part, silicone oil suds-stabilizing agent AK-8803 is 0.8 part and stirs with viscosity-depression agent diethylene glycol monoethyl ether 8 parts, prepare component A,
B component is poly methylene poly phenyl poly isocyanate.
By the proportional sampling of component A, B component 1:1 or 1:1.17 in mass ratio by volume, application apparatus is pneumatic Double-liquid mud-injection pump and corollary apparatus thereof; Total mass needed for test request calculates required each constituent mass, sufficient for mixing material is poured into self-vulcanizing in Standard Module, tests mechanical index after cooling.Adhesive property presses the strict sample preparation of standard-required, puts into 25 DEG C of baking ovens and preserves test after at least 3 hours.
Set time (25 DEG C): 80 seconds
Viscosity (25 DEG C): 178mPa.s
Ultimate compression strength: 78.3MPa
Tensile strength: 34.1MPa
Shear strength: 23.6MPa
Cohesive strength: 6.5MPa
Flame retardant resistance: spirit lamp experiment flaming combustion 1.5 seconds.
Embodiment 14
The preparation method of component A is as follows:
Be 2 ~ 4 by polyether glycol A(functionality, molecular weight is 800 ~ 1200, viscosity is 400 ~ 1000mPa.s) be 41 parts, polyether glycol B(functionality is 2 ~ 4, molecular weight is 500 ~ 800, viscosity is 300 ~ 600mPa.s) be 25 parts, polyether glycol C(functionality is 3 ~ 5, molecular weight is 200 ~ 400, viscosity is 1000 ~ 1500mPa.s) be 7 parts of mixing, to add fire retardant A dimethyl methyl phosphonate be 12 parts and fire retardant B tri-(2-chloroethyl) phosphoric acid ester is 7.15 parts of mixing, finally add amines catalyst five methyl diethylentriamine 0.35 part, tin class catalyst dibutyltin dilaurylate 0.5 part, silicone oil suds-stabilizing agent H-3612 is 1.0 parts and stirs with viscosity-depression agent diethylene glycol monoethyl ether 6 parts, prepare component A,
B component is poly methylene poly phenyl poly isocyanate.
By the proportional sampling of component A, B component 1:1 or 1:1.17 in mass ratio by volume, application apparatus is pneumatic Double-liquid mud-injection pump and corollary apparatus thereof; Total mass needed for test request calculates required each constituent mass, sufficient for mixing material is poured into self-vulcanizing in Standard Module, tests mechanical index after cooling.Adhesive property presses the strict sample preparation of standard-required, puts into 25 DEG C of baking ovens and preserves test after at least 3 hours.
Set time (25 DEG C): 72 seconds
Viscosity (25 DEG C): 189mPa.s
Ultimate compression strength: 76.8MPa
Tensile strength: 32.5MPa
Shear strength: 23.1MPa
Cohesive strength: 6.4MPa
Flame retardant resistance: spirit lamp experiment flaming combustion 1.5 seconds.
Above-mentioned is can understand and apply the invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to embodiment here, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (9)
1. a urethane reinforcement material, is characterized in that, comprises component A and B component,
Described component A comprises the component of following weight part:
Polyether glycol A is 20 ~ 45 parts, and polyether glycol B is 25 ~ 55 parts, and polyether glycol C is 5 ~ 10 parts, fire retardant A is 5 ~ 15 parts, and fire retardant B is 5 ~ 10 parts, and amines catalyst is 0.2 ~ 0.5 part, tin class catalyzer is 0.1 ~ 0.5 part, and suds-stabilizing agent is 0.5 ~ 1.0 part;
Described B component is poly methylene poly phenyl poly isocyanate;
The functionality of described polyether glycol A is 2 ~ 4, and molecular weight is 800 ~ 1200, and viscosity is 400 ~ 1000mPa.s;
The functionality of described polyether glycol B is 2 ~ 4, and molecular weight is 500 ~ 800, and viscosity is 300 ~ 600mPa.s;
The functionality of described polyether glycol C is 3 ~ 5, and molecular weight is 200 ~ 400, and viscosity is 1000 ~ 1500mPa.s.
2. urethane reinforcement material according to claim 1, is characterized in that, described urethane reinforcement material also comprises viscosity-depression agent 3 ~ 8 parts.
3. urethane reinforcement material according to claim 2, is characterized in that, described viscosity-depression agent is diethylene glycol monoethyl ether.
4. urethane reinforcement material according to claim 1 and 2, is characterized in that, described fire retardant A is dimethyl methyl phosphonate;
Described fire retardant B is three (2-chloroethyl) phosphoric acid ester or three (2-chloropropyl) phosphoric acid ester.
5. urethane reinforcement material according to claim 1 and 2, is characterized in that, described tin class catalyzer is dibutyl tin laurate;
Described amines catalyst is gel-like catalyzer or foaming kind catalyzer.
6. urethane reinforcement material according to claim 5, is characterized in that, described gel-like catalyzer is dimethylcyclohexylamine;
Described foaming kind catalyzer is five methyl diethylentriamine.
7. urethane reinforcement material according to claim 1 and 2, is characterized in that, described suds-stabilizing agent is silicone oil suds-stabilizing agent, uses the trade mark to be AK-8803, AK-8805 or H-3612;
Described poly methylene poly phenyl poly isocyanate is brown transparent liquid, and viscosity is 150 ~ 250mPa.s ,-NCO (wt%) is 30.5 ~ 32%;
The volume ratio of described component A and B component is 1:1 or mass ratio is 1:1.17.
8. the preparation method of the arbitrary described urethane reinforcement material of claim 1,4 ~ 7, is characterized in that, comprise the following steps:
The preparation method of described component A is as follows:
Be 20 ~ 45 parts by polyether glycol A, polyether glycol B is 25 ~ 55 parts, polyether glycol C is 5 ~ 10 parts of mixing, to add fire retardant A be 5 ~ 15 parts and fire retardant B is 5 ~ 10 parts of mixing, finally add that amines catalyst is 0.2 ~ 0.5 part, tin class catalyzer is that 0.1 ~ 0.5 part and suds-stabilizing agent are 0.5 ~ 1.0 part and stir, prepare component A;
Component A and the B component of to be 1:1 or mass ratio by volume ratio be 1:1.17 mix, solidify, and obtain urethane reinforcement material.
9. the preparation method of the arbitrary described urethane reinforcement material of claim 2 ~ 7, is characterized in that, comprise the following steps:
The preparation method of described component A is as follows:
Be 20 ~ 45 parts by polyether glycol A, polyether glycol B is 25 ~ 55 parts, polyether glycol C is 5 ~ 10 parts of mixing, to add fire retardant A be 5 ~ 15 parts and fire retardant B is 5 ~ 10 parts of mixing, finally add that amines catalyst is 0.2 ~ 0.5 part, tin class catalyzer is 0.1 ~ 0.5 part, suds-stabilizing agent is that 0.5 ~ 1.0 part and viscosity-depression agent are 3 ~ 8 parts and stir, prepare component A;
Component A and the B component of to be 1:1 or mass ratio by volume ratio be 1:1.17 mix, solidify, and obtain urethane reinforcement material.
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| CN105330814A (en) * | 2014-08-06 | 2016-02-17 | 上海茨夫新型建筑材料有限公司 | Polyurethane reinforcing material for reinforcing coal and rock mass in coal mine |
| CN104498004A (en) * | 2014-11-27 | 2015-04-08 | 山东一诺威新材料有限公司 | Chemical grouting material for coal-rock mass water shutoff and reinforcement and preparation method thereof |
| CN104448199B (en) * | 2014-12-19 | 2017-08-25 | 淄博正大聚氨酯有限公司 | Polyurethane elastomer sleeper and preparation method thereof |
| CN104479097B (en) * | 2014-12-30 | 2017-04-05 | 上海东大化学有限公司 | A kind of combined polyether, the feedstock composition of polyurethane reinforcement material and preparation method |
| CN106432685A (en) * | 2016-09-29 | 2017-02-22 | 合肥工业大学 | All-water-foamed and high-strength polyurethane grouting uplift material with high construction environment adaptability and low grout viscosity and preparation method of polyurethane grouting uplift material |
| CN107312158A (en) * | 2017-07-18 | 2017-11-03 | 合肥广能新材料科技有限公司 | Polyurethane foam external-wall heat-insulation material and preparation method thereof |
| CN108715682B (en) * | 2018-06-14 | 2021-03-30 | 山西凝固力新型材料股份有限公司 | Mining organic reinforcing material and preparation method thereof |
| CN111268941A (en) * | 2019-05-03 | 2020-06-12 | 石家庄国盛矿业科技有限公司 | Novel organic polymer double-liquid type grouting material for coal mine reinforcing coal rock mass |
| CN111303366A (en) * | 2020-03-26 | 2020-06-19 | 中煤科工集团重庆研究院有限公司 | Halogen-free flame-retardant organic polymer grouting reinforcement material and preparation method thereof |
| CN112142946A (en) * | 2020-08-21 | 2020-12-29 | 煤炭科学技术研究院有限公司 | Coal mine reinforcing material prepared from vegetable oil polyalcohol and preparation method thereof |
| CN112142950A (en) * | 2020-08-21 | 2020-12-29 | 煤炭科学技术研究院有限公司 | High-performance coal mine reinforcing material and preparation method thereof |
| CN112175570B (en) * | 2020-09-30 | 2022-04-29 | 有行鲨鱼（上海）科技股份有限公司 | Polyurethane adhesive and preparation method thereof |
| CN112979920A (en) * | 2021-02-25 | 2021-06-18 | 山西威瑞森环境技术有限公司 | Mining low-temperature foaming material and preparation method thereof |
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Effective date of registration: 20220117 Address after: 271400 economic and Technological Development Zone, Ningyang County, Tai'an City, Shandong Province (south of fujialou village to the west of national highway 104) Patentee after: Shandong anleng New Material Technology Co.,Ltd. Address before: 271000 North of Fengxiang Road, South High-tech Zone, Tai'an City, Shandong Province Patentee before: UROICA MINING SECURITY ENGINEERING CO.,LTD. |