CN110483718A - A kind of carbon fiber modifying no-solvent polyurethane surface layer resin - Google Patents
A kind of carbon fiber modifying no-solvent polyurethane surface layer resin Download PDFInfo
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- CN110483718A CN110483718A CN201910771280.9A CN201910771280A CN110483718A CN 110483718 A CN110483718 A CN 110483718A CN 201910771280 A CN201910771280 A CN 201910771280A CN 110483718 A CN110483718 A CN 110483718A
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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
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K7/00—Use of ingredients characterised by shape
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- C08K3/20—Oxides; Hydroxides
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Abstract
The invention belongs to field of compound material, especially a kind of carbon fiber modifying no-solvent polyurethane surface layer resin, it is poor for existing heat resistance, the low problem of thermal decomposition temperature, the short problem of product service life, it is proposed that following solution, including major ingredient and auxiliary material, the major ingredient includes resin, carbon fiber, inorganic solvent, polyalcohol, and the auxiliary material includes crosslinking agent, stabilizer, curing agent, defoaming agent, oxidant and mixing addition filler.It is mixed by using epoxy resin, polyamides resin and phenolic resin with carbon fiber, and adding corresponding oxidant reacts it sufficiently, increase the surface area of carbon fiber, the surface chemistry of carbon fiber is improved simultaneously, the oxygen-containing groups such as carboxyl, the hydroxyl of carbon fiber surface are significantly increased, low temperature, the high-temperature durable performance of finished product can be greatly improved preparing product after, while increase the anticorrosion performance of product.
Description
Technical field
The present invention relates to technical field of composite materials more particularly to a kind of carbon fiber modifying no-solvent polyurethane surface layer trees
Rouge.
Background technique
Polyurethane material is a kind of synthetic material between rubber and plastics, have high mechanical strength, chemical inertness,
A series of excellent performances such as high abrasion, cryogenic property, adhesive property and elasticity is good, but itself there is poor heat resistance, soft
Change the disadvantages such as low with thermal decomposition temperature, with the development of science and technology and the expansion of application, enhancing modification need to be carried out to polyurethane, raising
Its performance.Therefore, it is dedicated to developing important class of the compound polyurethane material as polyurethane field research of Good Heat-resistance
Topic.
The patent of invention of CN201610128326 provides a kind of modified carbon fiber compound polyurethane material and its preparation side
Method can effectively improve the flexibility and shock resistance of composite material, carbon fiber, sky by polyolefin block formula copolymer
Heart glass microballoon under the crosslinking of crosslinking agent, can with stable dispersion in the composite, thus greatly improve material toughness and
Intensity, the composite material being prepared is not easy to crack, and the composite material and preparation method thereof is simple, and mild condition is at low cost.
But this kind of composite material the problem of being used in life products, is, although toughness and intensity increase,
But very good solution heat resistance is not poor, the low problem of thermal decomposition temperature, product service life is short.
Summary of the invention
A kind of carbon fiber modifying no-solvent polyurethane surface layer resin proposed by the present invention, it is poor to solve heat resistance, heat point
Solve the low problem of temperature, the short problem of product service life.
To achieve the goals above, present invention employs following technical solutions:
A kind of carbon fiber modifying no-solvent polyurethane surface layer resin, including major ingredient and auxiliary material, the major ingredient include resin, carbon fiber
Dimension, inorganic solvent, polyalcohol, the auxiliary material include that crosslinking agent, stabilizer, curing agent, defoaming agent, oxidant and mixing addition are filled out
Material, wherein each ingredient uses following proportion: 30-45 parts of resin, 20-25 parts of carbon fiber, inorganic solvent 15-20 according to mass fraction
Part, 15-25 parts of polyalcohol, 2-4 parts of crosslinking agent, 3-5 parts of stabilizer, 1-3 parts of curing agent, 1-2 parts of defoaming agent, 3-5 parts of oxidant,
Filler 4-6 parts of mixing addition
Preferably, the resin includes epoxy resin, polyamides resin and phenolic resin, the epoxy resin, polyamides resin and phenol
The ratio of urea formaldehyde is 3:2:1.
Preferably, the polyalcohol be oligomer dihydric alcohol, organosilicon polyalcohol, polyester polyol, polyether polyol its
In one or more mixture, the inorganic solvent be sulfuric acid, nitric acid, liquid sulfur dioxide, thionyl chloride, chlorosulfuric acid wherein
One or more mixtures.
Preferably, the curing agent is TDI, IPDI, HDI and IPDI isocyanurate curing agent one or more of them
Mixture, the mixing addition filler are mixed by magnesia and aluminium oxide, and the ratio of the magnesia and aluminium oxide is 2:
3。
Preferably, the present invention also provides a kind of preparation method of carbon fiber modifying no-solvent polyurethane surface layer resin, tools
Preparation step are as follows:
Step 1: reaction kettle is dried, and is heated, is maintained the temperature at then to polyalcohol is added in reaction kettle
It after 110-130 DEG C of continuous heating 1-2h, is dehydrated under 0.05-0.1MPa vacuum condition, after dehydration completion into reaction kettle
Curing agent, defoaming agent, crosslinking agent and stabilizer are added, and is reduced to 65-95 DEG C to react temperature of reaction kettle, reaction is completed
After obtain material A；
Step 2: resin being added in another reaction kettle and is heated, and heating temperature is maintained at 70-90 DEG C, and into reaction kettle
Carbon fiber is added, carbon fiber is uniformly immersed in resin and is heated, material is uninterruptedly stirred in heating process,
Material B is obtained after heating 3-4h；
Step 3: material A is added slowly in material B and carries out that heating is sufficiently stirred, heating temperature is maintained at 130-160
DEG C, oxidant and mixing addition filler are added in heating process, while uninterrupted stirring is carried out to reaction kettle and removes bubble；
Step 4: reaction kettle being maintained at 120 DEG C and solidifies 1h, obtains finished product materials, is then injected in mold at 2-4MPa
Compression moulding obtains carbon fiber modifying no-solvent polyurethane surface layer resin.
Preferably, reaction kettle adds carbon fiber, material A in the step 3 after heating 1-3h to resin in the step 2
Filler is added with adding oxidant after material B agitating and heating 2h and mixing.
Compared with prior art, the beneficial effects of the present invention are:
1, it is mixed by using epoxy resin, polyamides resin and phenolic resin with carbon fiber in the present invention, and adds corresponding oxygen
Agent reacts it sufficiently, increases the surface area of carbon fiber, while improving the surface chemistry of carbon fiber, carbon fiber surface
The oxygen-containing groups such as carboxyl, the hydroxyl in face are significantly increased, can the low temperature for preparing product after and greatly improving finished product,
High-temperature durable performance, while increasing the anticorrosion performance of product；
2, it is mixed, can be effectively increased after material forming strong inside it with resin by addition mixing addition filler in the present invention
Degree, the filler being mixed by magnesia and aluminium oxide can effectively increase the tearing strength of product, while increase anti-oxidant effect
Fruit, water resistance also increase；
3, the present invention, can be simultaneously in different reaction kettles by carrying out hybrid process again after processing polyalcohol and resin respectively
It is middle to carry out different procedure of processings, high in machining efficiency, saving production cost.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.
Embodiment one:
A kind of carbon fiber modifying no-solvent polyurethane surface layer resin, including major ingredient and auxiliary material, the major ingredient include resin, carbon fiber
Dimension, inorganic solvent, polyalcohol, the auxiliary material include that crosslinking agent, stabilizer, curing agent, defoaming agent, oxidant and mixing addition are filled out
Material, wherein each ingredient uses following proportion: 30 parts of resin, 20 parts of carbon fiber, 15 parts of inorganic solvent, polyalcohol according to mass fraction
15 parts, 2 parts of crosslinking agent, 3 parts of stabilizer, 1 part of curing agent, 1 part of defoaming agent, 3 parts of oxidant, 4 parts of filler of mixing addition.
The resin includes epoxy resin, polyamides resin and phenolic resin, the epoxy resin, polyamides resin and phenolic aldehyde tree
The ratio of rouge is 3:2:1.
The polyalcohol be oligomer dihydric alcohol, organosilicon polyalcohol, polyester polyol, polyether polyol it is one of or
A variety of mixtures, the inorganic solvent are sulfuric acid, nitric acid, liquid sulfur dioxide, thionyl chloride, chlorosulfuric acid one of which or more
The mixture of kind.
The curing agent is the mixture of TDI, IPDI, HDI and IPDI isocyanurate curing agent one or more of them,
The mixing addition filler is mixed by magnesia and aluminium oxide, and the ratio of the magnesia and aluminium oxide is 2:3.
The present invention also provides a kind of preparation method of carbon fiber modifying no-solvent polyurethane surface layer resin, specific preparation step
Suddenly are as follows:
Step 1: reaction kettle is dried, and is heated, is maintained the temperature at then to polyalcohol is added in reaction kettle
After 110 DEG C of continuous heating 2h, be dehydrated under 0.05MPa vacuum condition, dehydration complete after into reaction kettle add curing agent,
Defoaming agent, crosslinking agent and stabilizer, and it is reduced to 65 DEG C to react temperature of reaction kettle, material A is obtained after the reaction was completed；
Step 2: resin being added in another reaction kettle and is heated, and heating temperature is maintained at 70 DEG C, and reaction kettle heats resin
Carbon fiber is added after 1h, carbon fiber is uniformly immersed in resin and is heated, and material is carried out in heating process uninterrupted
Stirring obtains material B after heating 4h；
Step 3: material A being added slowly in material B and be sufficiently stirred heating, and heating temperature is maintained at 130 DEG C, object
Oxidant and mixing addition filler are added after expecting A and material B agitating and heating 2h, while uninterruptedly stirring is carried out to reaction kettle and is removed
Bubble；
Step 4: reaction kettle being maintained at 120 DEG C and solidifies 1h, obtains finished product materials, and mold internal pressure is then injected at 2MPa
Type is made, obtains carbon fiber modifying no-solvent polyurethane surface layer resin.
Embodiment two:
A kind of carbon fiber modifying no-solvent polyurethane surface layer resin, including major ingredient and auxiliary material, the major ingredient include resin, carbon fiber
Dimension, inorganic solvent, polyalcohol, the auxiliary material include that crosslinking agent, stabilizer, curing agent, defoaming agent, oxidant and mixing addition are filled out
Material, wherein each ingredient uses following proportion: 45 parts of resin, 25 parts of carbon fiber, 20 parts of inorganic solvent, polyalcohol according to mass fraction
25 parts, 4 parts of crosslinking agent, 5 parts of stabilizer, 3 parts of curing agent, 2 parts of defoaming agent, 5 parts of oxidant, 6 parts of filler of mixing addition.
The resin includes epoxy resin, polyamides resin and phenolic resin, the epoxy resin, polyamides resin and phenolic aldehyde tree
The ratio of rouge is 3:2:1.
The polyalcohol be oligomer dihydric alcohol, organosilicon polyalcohol, polyester polyol, polyether polyol it is one of or
A variety of mixtures, the inorganic solvent are sulfuric acid, nitric acid, liquid sulfur dioxide, thionyl chloride, chlorosulfuric acid one of which or more
The mixture of kind.
The curing agent is the mixture of TDI, IPDI, HDI and IPDI isocyanurate curing agent one or more of them,
The mixing addition filler is mixed by magnesia and aluminium oxide, and the ratio of the magnesia and aluminium oxide is 2:3.
The present invention also provides a kind of preparation method of carbon fiber modifying no-solvent polyurethane surface layer resin, specific preparation step
Suddenly are as follows:
Step 1: reaction kettle is dried, and is heated, is maintained the temperature at then to polyalcohol is added in reaction kettle
After 130 DEG C of continuous heating 1h, be dehydrated under 0.1MPa vacuum condition, dehydration complete after into reaction kettle add curing agent,
Defoaming agent, crosslinking agent and stabilizer, and it is reduced to 95 DEG C to react temperature of reaction kettle, material A is obtained after the reaction was completed；
Step 2: resin being added in another reaction kettle and is heated, and heating temperature is maintained at 90 DEG C, and reaction kettle heats resin
Carbon fiber is added after 3h, carbon fiber is uniformly immersed in resin and is heated, and material is carried out in heating process uninterrupted
Stirring obtains material B after heating 3h；
Step 3: material A being added slowly in material B and be sufficiently stirred heating, and heating temperature is maintained at 160 DEG C, object
Oxidant and mixing addition filler are added after expecting A and material B agitating and heating 2h, while uninterruptedly stirring is carried out to reaction kettle and is removed
Bubble；
Step 4: reaction kettle being maintained at 120 DEG C and solidifies 1h, obtains finished product materials, and mold internal pressure is then injected at 4MPa
Type is made, obtains carbon fiber modifying no-solvent polyurethane surface layer resin.
Embodiment three:
A kind of carbon fiber modifying no-solvent polyurethane surface layer resin, including major ingredient and auxiliary material, the major ingredient include resin, carbon fiber
Dimension, inorganic solvent, polyalcohol, the auxiliary material include that crosslinking agent, stabilizer, curing agent, defoaming agent, oxidant and mixing addition are filled out
Material, wherein each ingredient uses following proportion: 38 parts of resin, 23 parts of carbon fiber, 18 parts of inorganic solvent, polyalcohol according to mass fraction
20 parts, 3 parts of crosslinking agent, 4 parts of stabilizer, 2 parts of curing agent, 1.5 parts of defoaming agent, 4 parts of oxidant, 5 parts of filler of mixing addition.
Preferably, the resin includes epoxy resin, polyamides resin and phenolic resin, the epoxy resin, polyamides resin
Ratio with phenolic resin is 3:2:1.
The polyalcohol be oligomer dihydric alcohol, organosilicon polyalcohol, polyester polyol, polyether polyol it is one of or
A variety of mixtures, the inorganic solvent are sulfuric acid, nitric acid, liquid sulfur dioxide, thionyl chloride, chlorosulfuric acid one of which or more
The mixture of kind.
The curing agent is the mixture of TDI, IPDI, HDI and IPDI isocyanurate curing agent one or more of them,
The mixing addition filler is mixed by magnesia and aluminium oxide, and the ratio of the magnesia and aluminium oxide is 2:3.
The present invention also provides a kind of preparation method of carbon fiber modifying no-solvent polyurethane surface layer resin, specific preparation step
Suddenly are as follows:
Step 1: reaction kettle is dried, and is heated, is maintained the temperature at then to polyalcohol is added in reaction kettle
It after 120 DEG C of continuous heating 1.5h, is dehydrated under 0.08MPa vacuum condition, dehydration adds solidification into reaction kettle after completing
Agent, defoaming agent, crosslinking agent and stabilizer, and it is reduced to 80 DEG C to react temperature of reaction kettle, material is obtained after the reaction was completed
A；
Step 2: resin being added in another reaction kettle and is heated, and heating temperature is maintained at 80 DEG C, and is added into reaction kettle
Carbon fiber is uniformly immersed in resin and heats by carbon fiber, is uninterruptedly stirred in heating process to material, heating
Material B is obtained after 3.5h；
Step 3: material A being added slowly in material B and be sufficiently stirred heating, and heating temperature is maintained at 145 DEG C, adds
Oxidant and mixing addition filler are added in thermal process, while uninterrupted stirring is carried out to reaction kettle and removes bubble；
Step 4: reaction kettle being maintained at 120 DEG C and solidifies 1h, obtains finished product materials, and mold internal pressure is then injected at 3MPa
Type is made, obtains carbon fiber modifying no-solvent polyurethane surface layer resin.
Reaction kettle adds carbon fiber after heating 2h to resin in the step 2, and material A and material B are stirred in the step 3
Oxidant and mixing addition filler are added after mixing heating 2h.
Example IV:
By embodiment one, embodiment two and embodiment three, finished product obtained carries out quality testing respectively, and specific detection data is as follows:
By above-mentioned data, it can be concluded that, carbon fiber modifying no-solvent polyurethane surface layer resin provided by the invention makes preparing product
Low temperature, the high-temperature durable performance of finished product are greatly improved after, while increasing the anticorrosion performance of product, fully meet various automobiles
Interior trim uses.
Embodiment five:
Referring to above-described embodiment, various automotive interior products made from embodiment three and existing automotive interior product are carried out pair
Than test, test data is as follows:
| The present invention | Existing product | |
| Oxidization time (min) at 80 DEG C of microwave | 36 | 28 |
| Contact angle (°) when being aoxidized at 80 DEG C of microwave | 62 | 97 |
| Oxidization time (min) at 100 DEG C of microwave | 15 | 8 |
| Contact angle (°) when being aoxidized at 100 DEG C of microwave | 53 | 89 |
By above-mentioned data, it can be concluded that, carbon fiber modifying no-solvent polyurethane surface layer resin provided by the invention is preparing various vapour
The antioxygenic property of product can be obviously increased on in-car decorations product, improve product service life.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of carbon fiber modifying no-solvent polyurethane surface layer resin, including major ingredient and auxiliary material, which is characterized in that the major ingredient packet
Resin, carbon fiber, inorganic solvent, polyalcohol are included, the auxiliary material includes crosslinking agent, stabilizer, curing agent, defoaming agent, oxidant
With mixing add filler, wherein each ingredient according to mass fraction use following proportion: 30-45 parts of resin, 20-25 parts of carbon fiber,
15-20 parts of inorganic solvent, 15-25 parts of polyalcohol, 2-4 parts of crosslinking agent, 3-5 parts of stabilizer, 1-3 parts of curing agent, defoaming agent 1-2
Part, 3-5 parts of oxidant, filler 4-6 parts of mixing addition.
2. a kind of carbon fiber modifying no-solvent polyurethane surface layer resin according to claim 1, which is characterized in that the tree
Rouge includes epoxy resin, polyamides resin and phenolic resin, and the ratio of the epoxy resin, polyamides resin and phenolic resin is 3:2:
1。
3. a kind of carbon fiber modifying no-solvent polyurethane surface layer resin according to claim 1, which is characterized in that described more
First alcohol be oligomer dihydric alcohol, organosilicon polyalcohol, polyester polyol, polyether polyol one or more of them mixture,
The inorganic solvent be sulfuric acid, nitric acid, liquid sulfur dioxide, thionyl chloride, chlorosulfuric acid one or more of them mixture.
4. a kind of carbon fiber modifying no-solvent polyurethane surface layer resin according to claim 1, which is characterized in that described solid
Agent is the mixture of TDI, IPDI, HDI and IPDI isocyanurate curing agent one or more of them, and the mixing addition is filled out
Material is mixed by magnesia and aluminium oxide, and the ratio of the magnesia and aluminium oxide is 2:3.
5. a kind of preparation side of carbon fiber modifying no-solvent polyurethane surface layer resin according to any one of claims 1-4
Method, which is characterized in that specific preparation step are as follows:
Step 1: reaction kettle is dried, and is heated, is maintained the temperature at then to polyalcohol is added in reaction kettle
It after 110-130 DEG C of continuous heating 1-2h, is dehydrated under 0.05-0.1MPa vacuum condition, after dehydration completion into reaction kettle
Curing agent, defoaming agent, crosslinking agent and stabilizer are added, and is reduced to 65-95 DEG C to react temperature of reaction kettle, reaction is completed
After obtain material A；
Step 2: resin being added in another reaction kettle and is heated, and heating temperature is maintained at 70-90 DEG C, and into reaction kettle
Carbon fiber is added, carbon fiber is uniformly immersed in resin and is heated, material is uninterruptedly stirred in heating process,
Material B is obtained after heating 3-4h；
Step 3: material A is added slowly in material B and carries out that heating is sufficiently stirred, heating temperature is maintained at 130-160
DEG C, oxidant and mixing addition filler are added in heating process, while uninterrupted stirring is carried out to reaction kettle and removes bubble；
Step 4: reaction kettle being maintained at 120 DEG C and solidifies 1h, obtains finished product materials, is then injected in mold at 2-4MPa
Compression moulding obtains carbon fiber modifying no-solvent polyurethane surface layer resin.
6. a kind of preparation method of carbon fiber modifying no-solvent polyurethane surface layer resin according to claim 5, feature
It is, reaction kettle adds carbon fiber after heating 1-3h to resin in the step 2, and material A and material B are stirred in the step 3
Oxidant is added after mixing heating 2h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104086738A (en) * | 2014-07-07 | 2014-10-08 | 旭川化学（苏州）有限公司 | Solvent-free environment-friendly polyurethane automobile leather surface resin as well as preparation method and application thereof |
| CN106397722A (en) * | 2016-08-31 | 2017-02-15 | 合肥安利聚氨酯新材料有限公司 | Carbon fiber modified non-solvent polyurethane surface layer resin for sports shoe leather, as well as preparation method and application of carbon fiber modified non-solvent polyurethane surface layer resin |
| CN110066373A (en) * | 2019-03-19 | 2019-07-30 | 合肥科天水性科技有限责任公司 | Use for synthetic leather solvent-free polyurethane resin and preparation method thereof and the application in aqueous/no-solvent polyurethane synthetic leather |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104086738A (en) * | 2014-07-07 | 2014-10-08 | 旭川化学（苏州）有限公司 | Solvent-free environment-friendly polyurethane automobile leather surface resin as well as preparation method and application thereof |
| CN106397722A (en) * | 2016-08-31 | 2017-02-15 | 合肥安利聚氨酯新材料有限公司 | Carbon fiber modified non-solvent polyurethane surface layer resin for sports shoe leather, as well as preparation method and application of carbon fiber modified non-solvent polyurethane surface layer resin |
| CN110066373A (en) * | 2019-03-19 | 2019-07-30 | 合肥科天水性科技有限责任公司 | Use for synthetic leather solvent-free polyurethane resin and preparation method thereof and the application in aqueous/no-solvent polyurethane synthetic leather |
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