CN109134821A - A kind of flame retardant thermoplastic polyurethane elastomer and preparation method thereof - Google Patents
A kind of flame retardant thermoplastic polyurethane elastomer and preparation method thereof Download PDFInfo
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- CN109134821A CN109134821A CN201810769116.XA CN201810769116A CN109134821A CN 109134821 A CN109134821 A CN 109134821A CN 201810769116 A CN201810769116 A CN 201810769116A CN 109134821 A CN109134821 A CN 109134821A
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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
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
-
- 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
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
-
- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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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
- C08K5/5313—Phosphinic compounds, e.g. R2=P(:O)OR'
-
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/16—Solid spheres
- C08K7/18—Solid spheres inorganic
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a kind of flame retardant thermoplastic polyurethane elastomers, including the following ingredients formed by weight: isophorone diisocyanate: 80-85 parts, polytetrahydrofuran ether glycol: 20-30 parts, organo montmorillonite: 20-30 parts, mixing fire retardant: 10-15 parts, mixed chain extender: 8-10 parts and carbon ball (CNS): 3-5 parts.The present invention can more effectively prevent the propagation of heat and oxygen using the flame retardant thermoplastic polyurethane elastomer of mixing fire retardant preparation, thus have superior anti-flammability.
Description
Technical field
The invention belongs to polymeric material fields, and in particular to a kind of flame retardant thermoplastic polyurethane elastomer and its preparation side
Method.
Background technique
Thermoplastic polyurethane (TPU) be obtained by diisocyanate, chain extender and macromolecular diol polymerization reaction it is linear
Or lightly crosslinked high molecular polymer, it is a kind of elastic material between plastics and rubber, there is excellent wearability
Energy, physical mechanical property outstanding, fabulous oil resistance, wider temperature use scope, wider hardness range are good
Shock attenuation result, excellent tear resistance, therefore be widely used in social every profession and trade.But due to easy firing, burning is released
The toxic gases such as hydrogen cyanide are put, therefore there are security risks at it.
Summary of the invention
It is an object of the invention to overcome the technical problem present on, a kind of flame-proof thermoplastic polyurethane elasticity is provided
Body.
To achieve the above object, the technical scheme is that in the following manner realizing:
A kind of flame retardant thermoplastic polyurethane elastomer, including the following ingredients formed by weight: two isocyanide of isophorone
Acid esters: 80-85 parts, polytetrahydrofuran ether glycol: 20-30 parts, organo montmorillonite: 20-30 parts, mixing fire retardant: 10-15 parts,
Mixed chain extender: 8-10 parts and carbon ball (CNS): 3-5 parts.
Further, the isophorone diisocyanate is 80 parts, 20 parts of polytetrahydrofuran ether glycol, organo montmorillonite
3 parts of 20 parts, 10 parts of fire retardant of mixing, 8 parts of mixed chain extender and carbon ball (CNS).
Further, the isophorone diisocyanate is 85 parts, 30 parts of polytetrahydrofuran ether glycol, organo montmorillonite
5 parts of 30 parts, 15 parts of fire retardant of mixing, 10 parts of mixed chain extender and carbon ball (CNS).
Further, the isophorone diisocyanate is 83 parts, 25 parts of polytetrahydrofuran ether glycol, organo montmorillonite
4 parts of 25 parts, 13 parts of fire retardant of mixing, 9 parts of mixed chain extender and carbon ball (CNS).
Further, the mixing fire retardant is by phosphor-containing flame-proof and the miscellaneous -10- phospho hetero phenanthrene-of 10- dihydro-9-oxy
10- oxide (DOPO) mixes, mixed proportion 3:7.
Further, the mixed chain extender by bis- (2- ethoxy) ethers (HQEE) of quinhydrones, 1,4-butanediol (BDO) and
Hexafluoro bisphenol-a mixes, mixed proportion 3:3:4.
The present invention also provides a kind of method for preparing fire retardant thermoplastic polyurethane elastomer, comprising the following steps:
S1: under the conditions of high temperature, 0.1MPa, by polytetrahydrofuran ether glycol vacuum dehydration 1.5-2h；
S2: suitable polytetrahydrofuran ether glycol, isophorone diisocyanate, organo montmorillonite, carbon ball after dehydration are taken
(CNS) and mixing fire retardant be added to equipped with mechanical stirring, condensation reflux unit, thermometer four-hole boiling flask in, be warming up to 70
DEG C, it vacuumizes, is filled with nitrogen protection, after sustained response 1.5-2h, solvent dimethylformamide is added adjusts solid content and be
60wt% promotees the progress that reacts fully to reduce system viscosity；
S3: after isocyanate group mass fraction is stablized in performed polymer to be determined, being gradually heated to 100 DEG C, and mixing is added and expands
Chain agent is vigorously stirred reaction 2h, and vacuum outgas, then drying obtains flame-proof thermoplastic polyurethane mixture, to complete to prepare.
Further, the high temperature is 110-120 DEG C.
Further, the mixing fire retardant is by phosphor-containing flame-proof and the miscellaneous -10- phospho hetero phenanthrene-of 10- dihydro-9-oxy
10- oxide (DOPO) mixes, mixed proportion 3:7.
Further, the mixed chain extender by bis- (2- ethoxy) ethers (HQEE) of quinhydrones, 1,4-butanediol (BDO) and
Hexafluoro bisphenol-a mixes, mixed proportion 3:3:4.
The present invention has the advantages that through overtesting
1, the flame retardant thermoplastic polyurethane elastomer prepared using mixed chain extender, tensile strength and tearing strength obtain
It significantly improves.
2, using the flame retardant thermoplastic polyurethane elastomer of mixing fire retardant preparation, the biography of heat and oxygen can more effectively be prevented
It broadcasts, thus there is superior anti-flammability.
3, flame retardant thermoplastic polyurethane elastomer is made to have the function of not only enhancing but also toughening using organo montmorillonite.
Specific embodiment
The following describes the present invention in detail with reference to examples.
Embodiment one:
A kind of flame retardant thermoplastic polyurethane elastomer, including the following ingredients formed by weight: the isophorone two
Isocyanates is 80 parts, 20 parts of polytetrahydrofuran ether glycol, 20 parts of organo montmorillonite, mixes 10 parts of fire retardant, mixed chain extender 8
Part and 3 parts of carbon ball (CNS).The mixing fire retardant is by phosphor-containing flame-proof and the miscellaneous -10- phospho hetero phenanthrene-of 10- dihydro-9-oxy
10- oxide (DOPO) mixes, mixed proportion 3:7.The mixed chain extender is by bis- (2- ethoxy) ethers of quinhydrones
(HQEE), 1,4-butanediol (BDO) and hexafluoro bisphenol-a mix, mixed proportion 3:3:4.
Experimental result shows that carbon ball (CNS) is containing there are many hydroxyls can make carbon ball CNS with polyurethane molecular formation hydrogen bond)
Fine dispersion and the tensile property of compound polyurethane material is improved in polyurethane matrix, to improve the poly- ammonia of flame-proofed thermoplastic
The tensile property of ester elastomer.And carbon ball hinders the crystallization of polyurethane, to reduce flame-proof thermoplastic polyurethane elasticity
The elasticity modulus and lag damage of body.
The method for preparing fire retardant thermoplastic polyurethane elastomer, comprising the following steps:
S1: under the conditions of 110-120 DEG C, 0.1MPa, by polytetrahydrofuran ether glycol vacuum dehydration 1.5-2h；
S2: suitable polytetrahydrofuran ether glycol, isophorone diisocyanate, organo montmorillonite, carbon ball after dehydration are taken
(CNS) and mixing fire retardant be added to equipped with mechanical stirring, condensation reflux unit, thermometer four-hole boiling flask in, be warming up to 70
DEG C, it vacuumizes, is filled with nitrogen protection, after sustained response 1.5-2h, solvent dimethylformamide is added adjusts solid content and be
60wt% promotees the progress that reacts fully to reduce system viscosity；
S3: after isocyanate group mass fraction is stablized in performed polymer to be determined, being gradually heated to 100 DEG C, and mixing is added and expands
Chain agent is vigorously stirred reaction 2h, and vacuum outgas, then drying obtains flame-proof thermoplastic polyurethane mixture, to complete to prepare.
Wherein, the mixing fire retardant is by phosphor-containing flame-proof and the miscellaneous -10- phospho hetero phenanthrene -10- oxygen of 10- dihydro-9-oxy
Compound (DOPO) mixes, mixed proportion 3:7.
Wherein, the mixed chain extender is by bis- (2- ethoxy) ethers (HQEE) of quinhydrones, 1,4-butanediol (BDO) and hexafluoro
Bisphenol-A mixes, mixed proportion 3:3:4.
Embodiment two:
A kind of flame retardant thermoplastic polyurethane elastomer, including the following ingredients formed by weight: the isophorone two
Isocyanates is 85 parts, 30 parts of polytetrahydrofuran ether glycol, 30 parts of organo montmorillonite, mixes 15 parts of fire retardant, mixed chain extender
10 parts and 5 parts of carbon ball (CNS).The mixing fire retardant is by phosphor-containing flame-proof and the miscellaneous -10- phospho hetero phenanthrene-of 10- dihydro-9-oxy
10- oxide (DOPO) mixes, mixed proportion 3:7.The mixed chain extender is by bis- (2- ethoxy) ethers of quinhydrones
(HQEE), 1,4-butanediol (BDO) and hexafluoro bisphenol-a mix, mixed proportion 3:3:4.Preparation method and above-mentioned reality
It is identical to apply example one.
Embodiment three:
A kind of flame retardant thermoplastic polyurethane elastomer, including the following ingredients formed by weight: the isophorone two
Isocyanates is 85 parts, 30 parts of polytetrahydrofuran ether glycol, 30 parts of organo montmorillonite, mixes 15 parts of fire retardant, mixed chain extender
10 parts and 5 parts of carbon ball (CNS).The mixing fire retardant is by phosphor-containing flame-proof and the miscellaneous -10- phospho hetero phenanthrene-of 10- dihydro-9-oxy
10- oxide (DOPO) mixes, mixed proportion 3:7.The mixed chain extender is by bis- (2- ethoxy) ethers of quinhydrones
(HQEE), 1,4-butanediol (BDO) and hexafluoro bisphenol-a mix, mixed proportion 3:3:4.Preparation method and above-mentioned reality
It is identical to apply example one.
Finally, it should be noted that above embodiments are only to illustrate the present invention and not limit technology described in the invention
Scheme；Therefore, although this specification is referring to above-mentioned each embodiment, the present invention has been described in detail, this
Field it is to be appreciated by one skilled in the art that still can modify to the present invention or equivalent replacement；And all do not depart from this
The technical solution and its improvement of the spirit and scope of invention, should all cover within the scope of the claims of the present invention.
Claims (10)
1. a kind of flame retardant thermoplastic polyurethane elastomer, which is characterized in that including the following ingredients formed by weight: different Fo Er
Ketone diisocyanate: 80-85 parts, polytetrahydrofuran ether glycol: 20-30 parts, organo montmorillonite: 20-30 parts, mixing fire retardant:
10-15 parts, mixed chain extender: 8-10 parts and carbon ball (CNS): 3-5 parts.
2. flame retardant thermoplastic polyurethane elastomer according to claim 1, which is characterized in that two isocyanide of isophorone
Acid esters be 80 parts, 20 parts of polytetrahydrofuran ether glycol, 20 parts of organo montmorillonite, mixing 10 parts of fire retardant, 8 parts of mixed chain extender and
3 parts of carbon ball (CNS).
3. flame retardant thermoplastic polyurethane elastomer according to claim 1, which is characterized in that two isocyanide of isophorone
Acid esters is 85 parts, 30 parts of polytetrahydrofuran ether glycol, 30 parts of organo montmorillonite, mixes 15 parts of fire retardant, 10 parts of mixed chain extender
With 5 parts of carbon ball (CNS).
4. flame retardant thermoplastic polyurethane elastomer according to claim 1, which is characterized in that two isocyanide of isophorone
Acid esters be 83 parts, 25 parts of polytetrahydrofuran ether glycol, 25 parts of organo montmorillonite, mixing 13 parts of fire retardant, 9 parts of mixed chain extender and
4 parts of carbon ball (CNS).
5. flame retardant thermoplastic polyurethane elastomer according to claim 1 to 4, which is characterized in that the mixing is fire-retardant
Agent is mixed by phosphor-containing flame-proof and the miscellaneous -10- phospho hetero phenanthrene -10- oxide (DOPO) of 10- dihydro-9-oxy, mixing ratio
Example is 3:7.
6. flame retardant thermoplastic polyurethane elastomer according to claim 1 to 4, which is characterized in that the mixing chain extension
Agent is mixed by bis- (2- ethoxy) ethers (HQEE) of quinhydrones, 1,4-butanediol (BDO) and hexafluoro bisphenol-a, and mixed proportion is
3:3:4。
7. a kind of method for preparing fire retardant thermoplastic polyurethane elastomer, which comprises the following steps:
S1: under the conditions of high temperature, 0.1MPa, by polytetrahydrofuran ether glycol vacuum dehydration 1.5-2h；
S2: suitable polytetrahydrofuran ether glycol, isophorone diisocyanate, organo montmorillonite, carbon ball (CNS) after dehydration are taken
With mixing fire retardant be added to equipped with mechanical stirring, condensation reflux unit, thermometer four-hole boiling flask in, be warming up to 70 DEG C, take out
Vacuum, is filled with nitrogen protection, and after sustained response 1.5-2h, it is 60wt% that solvent dimethylformamide, which is added, and adjusts solid content, with
System viscosity is reduced, the progress that reacts fully is promoted；
S3: after isocyanate group mass fraction is stablized in performed polymer to be determined, being gradually heated to 100 DEG C, mixed chain extender be added,
It is vigorously stirred reaction 2h, vacuum outgas, then drying obtains flame-proof thermoplastic polyurethane mixture, to complete to prepare.
8. method for preparing fire retardant thermoplastic polyurethane elastomer according to claim 7, which is characterized in that the high temperature
It is 110-120 DEG C.
9. method for preparing fire retardant thermoplastic polyurethane elastomer according to claim 7 or 8, which is characterized in that described
Fire retardant is mixed by phosphor-containing flame-proof and the mixing of 10- dihydro-9-oxy miscellaneous -10- phospho hetero phenanthrene -10- oxide (DOPO) and
At mixed proportion 3:7.
10. method for preparing fire retardant thermoplastic polyurethane elastomer according to claim 7 or 8, which is characterized in that described
Mixed chain extender is mixed by bis- (2- ethoxy) ethers (HQEE) of quinhydrones, 1,4-butanediol (BDO) and hexafluoro bisphenol-a, is mixed
Composition and division in a proportion example is 3:3:4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810769116.XA CN109134821A (en) | 2018-07-13 | 2018-07-13 | A kind of flame retardant thermoplastic polyurethane elastomer and preparation method thereof |
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| CN201810769116.XA CN109134821A (en) | 2018-07-13 | 2018-07-13 | A kind of flame retardant thermoplastic polyurethane elastomer and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110408190A (en) * | 2019-07-30 | 2019-11-05 | 湖北大学 | Preparation method, product and the purposes of ultraviolet resistance radiation carbon ball modified polyurethane |
| CN115012086A (en) * | 2022-06-07 | 2022-09-06 | 江阴市聚鑫花式线有限公司 | Fancy yarn dyed by vegetable dye and processing technology thereof |
| CN115029833A (en) * | 2022-06-07 | 2022-09-09 | 江阴市聚鑫花式线有限公司 | Flame-retardant fancy yarn and preparation process thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110408190A (en) * | 2019-07-30 | 2019-11-05 | 湖北大学 | Preparation method, product and the purposes of ultraviolet resistance radiation carbon ball modified polyurethane |
| CN115012086A (en) * | 2022-06-07 | 2022-09-06 | 江阴市聚鑫花式线有限公司 | Fancy yarn dyed by vegetable dye and processing technology thereof |
| CN115029833A (en) * | 2022-06-07 | 2022-09-09 | 江阴市聚鑫花式线有限公司 | Flame-retardant fancy yarn and preparation process thereof |
| CN115029833B (en) * | 2022-06-07 | 2024-02-06 | 江阴市聚鑫花式线有限公司 | Flame-retardant fancy yarn and preparation process thereof |
| CN115012086B (en) * | 2022-06-07 | 2024-02-06 | 江阴市聚鑫花式线有限公司 | Plant dye dyeing fancy yarn and processing technology thereof |
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