CN104927085B - A kind of multifunctional assistant and preparation method thereof and the application in polyamide compoiste material is prepared - Google Patents
A kind of multifunctional assistant and preparation method thereof and the application in polyamide compoiste material is prepared Download PDFInfo
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- CN104927085B CN104927085B CN201510329849.8A CN201510329849A CN104927085B CN 104927085 B CN104927085 B CN 104927085B CN 201510329849 A CN201510329849 A CN 201510329849A CN 104927085 B CN104927085 B CN 104927085B
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- multifunctional assistant
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Abstract
Application the invention provides a kind of multifunctional assistant and preparation method thereof and in polyamide compoiste material is prepared, the multifunctional assistant, it is made up of the raw material of following weight percentage：Maleic anhydride 35 50%, hexamethylene diamine 49.9 64%, antioxidant 0.05 3%.The preparation of described multifunctional assistant includes：It is first that hexamethylene diamine and antioxidant melting mixing is uniform, the maleic anhydride of melting is then added dropwise, multifunctional assistant is obtained after the completion of reaction.Multifunctional assistant of the present invention can be used as flow ability modifying agent, outward appearance modifying agent and fluorescent whitening agent to be used in polyamide compoiste material, the auxiliary agent realizes a kind of purpose of auxiliary agent multiple functions of polyamide compoiste material modifying process, reducing material property caused by a variety of auxiliary agents add reduces and cost increase problem, easily operated and implementation, it is easy to industrialization large-scale production, possesses wide application prospect.
Description
Technical field
The present invention relates to the auxiliary agent field for polyamide compoiste material, and in particular to a kind of multifunctional assistant and its preparation
Method and the application in polyamide compoiste material is prepared.
Background technology
Polyamide is also referred to as nylon, is linear thermoplastic's polymerization containing amide group constitutional repeating unit on molecular backbone
Thing, and nylon 6, nylon66 fiber are the two class base resins that yield is maximum in all Polyamide Engineering Plastics, purposes is most wide, it has
Outstanding mechanical strength, heat-resisting, oil resistant, weak acid resistant, alkaline-resisting and common solvent, electrical insulating property be good, nontoxic, odorless, weather-proof etc. excellent
Point, it is the irreplaceable high performance engineering plastics of automobile, electrical apparatus industry, still, due to nylon big amide group containing polarized, leads
Cause it that there is easily water suction the shortcomings that causing intensity decreases, therefore be generally required for strengthening it strong to improve its
Degree and heat aging property, meet the requirement under the conditions of various harsh environments.Due to reinforcer and other auxiliary agents plus
Enter, strengthen modified nylon composite materials typically can all occur mobility be deteriorated and product appearance glossiness reduce etc. ask
Topic, especially after glass fiber content is more than 30%, be easy to during the product for producing some structures to occur injection is discontented and product outside
See the situation of low in glossiness.In order to solve these problems, or material is possessed some properties, add various modified additives into
For simplest means.But a variety of auxiliary agents for being directed to difference in functionality and adding can increase the ratio of auxiliary agent in the composite
Example, reduces the mechanical property of composite, adds manufacturing cost, therefore a kind of exploitation of multifunctional assistant just seems particularly heavy
Will.
The Chinese invention patent application that application publication number is CN 104087067A (Application No. 201410086997.7) is public
A kind of made intaglio plate table print Antiforge fluorescent ink of novel fluorescent material has been opened, has been made up of the component of following weight percentage：
Terbium nitrate 0.2%~0.8%, 2,4- dihydroxy-benzoic acids 0.26%~1.04%, triethylamine 0.17%~0.68%, industrial wine
Essence 36.48%~38.37%, polyamide 25%~35%, n-butanol 25%~35%, slipping agent 0.5%, antiwear agents
0.5%.Wherein, will be blended under terbium nitrate, 2,4- dihydroxy-benzoic acids and triethylamine normal temperature in industrial alcohol, stirring 3~20
Minute, obtain fluorescent solutions.Although the fluorescent solutions can bring fluorescent effect to anti-forgery ink, by the fluorescent solutions application
Into polyamide compoiste material, polyamide compoiste material mobility can not be improved, can not also improve the outer of polyamide compoiste material
See.
Document " the different oxidizing influences to ethylenediamine fluorescence property " (Wang Shaofei etc., Hebei Science ＆ Technology Normal College
Journal, the 2nd phase of volume 26, in June, 2012) disclose 3 kinds of different oxidants ethylenediamine is aoxidized, and propose to use first
Hydrogen peroxide makees oxidant, and system research is carried out to the photoluminescent property of ethylenediamine solution after oxidation, the results showed that, hydrogen peroxide
Oxidation effectiveness is optimal, obtains fluorescence intensity highest.But the ethylenediamine solution after hydrogen peroxide oxidation is added to polyamide
In composite, polyamide compoiste material mobility can not be improved, can not also improve the outward appearance of polyamide compoiste material.
The content of the invention
Application the invention provides a kind of multifunctional assistant and preparation method thereof and in polyamide compoiste material is prepared,
The multifunctional assistant has while improves polyamide compoiste material mobility, improves composite outward appearance and possess and polyamide material
The function of material reaction fluorescent color.
The purpose of the present invention is achieved through the following technical solutions：
A kind of multifunctional assistant, it is made up of the raw material of following weight percentage：
Maleic anhydride 35%-50%；
Hexamethylene diamine 49.9%-64%；
Antioxidant 0.05%-3%；
Preferably, described multifunctional assistant, is made up of the raw material of following weight percentage：
Maleic anhydride 40%-45%；
Hexamethylene diamine 54.9%-59%；
Antioxidant 0.1%-1%.
Multifunctional assistant of the present invention, combined using the specific components of certain content, maleic anhydride, hexamethylene diamine and antioxidant are anti-
Small molecule amide compound should be generated, in polyamide compoiste material, can be crosslinked and react with the amide group in polyamide,
It is not only able to improve polyamide compoiste material mobility, improves composite outward appearance, additionally it is possible to reacts fluorescence with polyamide material
The function of coloring.
With weight, purity requirement >=99.9% of described maleic anhydride, and water content≤0.05%.
With weight, purity requirement >=99.9% of described hexamethylene diamine, and water content≤0.05%.
Described antioxidant is that antioxidant 1098, antioxidant 1010 one or both of are worked as.
The preparation method of described multifunctional assistant, comprises the following steps：
It is first that hexamethylene diamine and antioxidant melting mixing is uniform, the maleic anhydride of melting is then added dropwise, while in the process of dropwise addition
In be stirred continuously, multifunctional assistant is obtained after the completion of reaction.
The maleic anhydride of melting is being added dropwise, reaction, reaction generation small molecule amide compound can be produced, question response is completed
Afterwards, cooling crush obtains corresponding product, i.e. multifunctional assistant.
Application of the described multifunctional assistant in polyamide compoiste material is prepared.
Described polyamide compoiste material, it is made up of the raw material of following weight percentage：
Polyamide 50%-80%；
Multifunctional assistant 0.1%-10%；
Other components 10%-40%.
Further preferably, described polyamide compoiste material, it is made up of the raw material of following weight percentage：
The preparation method of described polyamide compoiste material, including：
After polyamide, composite antioxidant, multifunctional assistant are well mixed, double screw extruder is added from main feed hopper
In, by glass fibre from side position material hopper add double screw extruder in, after double screw extruder melting extrusion by water cooling,
Pelletizing and drying, obtain polyamide compoiste material；
The temperature of the melting extrusion of described double screw extruder is 215 DEG C~295 DEG C.
Further preferably, described polyamide compoiste material, it is made up of the raw material of following weight percentage：
After polyamide, fire retardant, fire retarding synergist, composite antioxidant, multifunctional assistant are well mixed, from main feeding material
Bucket is added in double screw extruder, glass fibre is added in double screw extruder from side position material hopper, through double screw extruder
By water cooling, pelletizing and drying after melting extrusion, polyamide compoiste material is obtained.
The temperature of the melting extrusion of described double screw extruder is 240 DEG C~290 DEG C.
Compared with prior art, the invention has the advantages that：
There is improvement simultaneously in polyamide compoiste material compared to other simple function auxiliary agents, multifunctional assistant of the present invention
Polyamide compoiste material mobility, improve composite outward appearance and possess the work(with polyamide material reaction in-situ fluorescent color
Can, solve the problems, such as that existing a variety of auxiliary agents add the mechanical property brought and reduced and cost increase.
Multifunctional assistant of the present invention can answer as flow ability modifying agent, outward appearance modifying agent and fluorescent whitening agent for polyamide
In condensation material, the auxiliary agent realizes a kind of purpose of auxiliary agent multiple functions of polyamide compoiste material modifying process, reduces a variety of
Material property caused by auxiliary agent adds reduces and cost increase problem, easily operated and implementation, is easy to industrialization large-scale production,
Possesses wide application prospect.
Embodiment
The purpose of the present invention, advantage and feature, it will be explained by the non-limitative illustration of following examples, these realities
It is only the prominent example using technical solution of the present invention to apply example, all technical sides formed using equivalent substitution or equivalent transformation
Case, within the claimed scope of the invention.
The not specified % of the embodiment of the present invention is weight percentage.
Embodiment 1
For the multifunctional assistant of polyamide compoiste material, it is particular in that：By the raw material system of following percentage by weight
Into：
Maleic anhydride 45.0%；
Hexamethylene diamine 54.9%；
Antioxidant 0.1%；
Above-mentioned multifunctional assistant, wherein：
The purity of described maleic anhydride is 99.9%, and water content is less than 0.04%.
The purity of described hexamethylene diamine is 99.9%, and water content is less than 0.04%.
Described antioxidant is antioxidant 1098.
The preparation process of multifunctional assistant is as follows：Hexamethylene diamine and antioxidant 1098 first are added into reactor fully melt
Melt, the maleic anhydride of melting is then added dropwise, is stirred vigorously simultaneously, react and generate small molecule amide compound, after the completion of question response,
Cooling crush obtains corresponding product, i.e. multifunctional assistant.
Further combined with polyamide compoiste material preparation process, by taking a kind of glass fiber reinforced materials of nylon 6 as an example, it has following
Percentage by weight raw material forms：PA6 (69%), alkali-free glass fiber (30%), composite antioxidant (0.5%), prepare by the above process
Multifunctional assistant of the present invention (0.5%).Wherein for the PA6 trades mark beautiful newly to reach M2800, alkali-free glass fiber is megalith 988A, compound
Antioxidant is antioxidant 1098 (0.25%), irgasfos 168 (0.25%).
The preparation method of above-mentioned polyamide compoiste material is：By nylon 6, composite antioxidant, the sheet prepared by the above process
Invention multifunctional assistant is added in homogenizer after 3000RPM mixing 1min, and twin-screw extrusion is added from main feed hopper
In machine, glass fibre (i.e. alkali-free glass fiber) is added in double screw extruder from side position material hopper, extruded through double screw extruder
Afterwards by water cooling, pelletizing and drying, polyamide compoiste material is obtained；First temperature of the double screw extruder from feed zone to head
Spend the temperature sections of Duan Zhi eight temperature setting be respectively 230 DEG C, 235 DEG C, 245 DEG C, 235 DEG C, 225 DEG C, 215 DEG C, 215 DEG C, 215
DEG C, the temperature of die head is 235 DEG C.
Polyamide compoiste material requires to carry out the detection of properties according to GB standards.
Embodiment 2
For the multifunctional assistant of polyamide compoiste material, it is particular in that：By the raw material system of following percentage by weight
Into：
Maleic anhydride 40.0%；
Hexamethylene diamine 59.9%；
Antioxidant 0.1%；
Above-mentioned multifunctional assistant, wherein：
The purity of described maleic anhydride is 99.9%, and water content is less than 0.04%.
The purity of described hexamethylene diamine is 99.9%, and water content is less than 0.04%.
Described antioxidant is antioxidant 1010.
The preparation process of multifunctional assistant is same as Example 1.
Further combined with polyamide compoiste material preparation process, by taking a kind of nylon66 fiber glass fiber reinforced materials as an example, its have with
Lower percentage by weight raw material composition：PA66 (69%), alkali-free glass fiber (30%), composite antioxidant (0.5%), make by the above process
Standby multifunctional assistant of the present invention (0.5%).Wherein the PA66 trades mark are Shen Ma groups EPR27, and alkali-free glass fiber is megalith 988A, multiple
Conjunction antioxidant is antioxidant 1098 (0.25%), irgasfos 168 (0.25%).
The preparation method of above-mentioned polyamide compoiste material is identical with composite material and preparation method thereof in embodiment 1, but this pair of spiral shell
First temperature section of the bar extruder from feed zone to head to the 8th temperature section temperature setting be respectively 290 DEG C, 295 DEG C, 285
DEG C, 265 DEG C, 255 DEG C, 255 DEG C, 255 DEG C, 255 DEG C, the temperature of die head is 285 DEG C.
Polyamide compoiste material requires to carry out the detection of properties according to GB standards.
Embodiment 3
For the multifunctional assistant of polyamide compoiste material, it is particular in that：By the raw material system of following percentage by weight
Into：
Maleic anhydride 45.0%；
Hexamethylene diamine 54.5%；
Antioxidant 0.5%；
Above-mentioned multifunctional assistant, wherein：
The purity of described maleic anhydride is 99.9%, and water content is less than 0.04%.
The purity of described hexamethylene diamine is 99.9%, and water content is less than 0.04%.
Described antioxidant is antioxidant 1010 (0.25%), antioxidant 1098 (0.25%) mixture.
The preparation process of multifunctional assistant is same as Example 1.
Further combined with polyamide compoiste material preparation process, by taking a kind of nylon66 fiber fiberglass reinforced fire retardant material as an example, its
It is made up of following percentage by weight raw material：PA66 (52%), alkali-free glass fiber (30%), fire retardant (13%), fire retarding synergist
4%, composite antioxidant (0.5%), the multifunctional assistant of the present invention (0.5%) prepared by the above process.The wherein PA66 trades mark are
Shen Ma groups EPR27, alkali-free glass fiber are megalith 988A, and fire retardant is the TDE in U.S. big lake, and fire retarding synergist is
The antimony oxide of Jinan Thailand star, composite antioxidant are antioxidant 1098 (0.25%), irgasfos 168 (0.25%).
The preparation method of above-mentioned polyamide compoiste material is：By nylon66 fiber, fire retardant, fire retarding synergist, composite antioxidant,
The multifunctional assistant of the present invention prepared by the above process is added in homogenizer after 3000RPM mixing 1min from main feeding material
Bucket is added in double screw extruder, glass fibre (i.e. alkali-free glass fiber) is added in double screw extruder from side position material hopper, warp
By water cooling, pelletizing and drying after double screw extruder extrusion, polyamide compoiste material is obtained；The double screw extruder is from charging
Section to head the first temperature section to the 8th temperature section temperature setting be respectively 280 DEG C, 285 DEG C, 275 DEG C, 255 DEG C, 245
DEG C, 245 DEG C, 245 DEG C, 245 DEG C, the temperature of die head is 265 DEG C.
Polyamide compoiste material requires to carry out the detection of properties according to GB standards.
Comparative example 1
By taking a kind of nylon66 fiber glass fiber reinforced materials as an example, it is made up of following percentage by weight raw material：PA66 (69.5%),
Alkali-free glass fiber (30%), wherein composite antioxidant (0.5%), the PA66 trades mark are Shen Ma groups EPR27, and alkali-free glass fiber is megalith
988A, composite antioxidant are antioxidant 1098 (0.25%), irgasfos 168 (0.25%).
The preparation method of above-mentioned polyamide compoiste material is identical with composite material and preparation method thereof in embodiment 2,
Polyamide compoiste material requires to carry out the detection of properties according to GB standards.
Comparative example 2
By taking a kind of nylon66 fiber fiberglass reinforced fire retardant material as an example, it is made up of following percentage by weight raw material：PA66
(52.5%), alkali-free glass fiber (30%), fire retardant (13%), fire retarding synergist 4%, composite antioxidant (0.5%).Wherein PA66
The trade mark is Shen Ma groups EPR27, and alkali-free glass fiber is megalith 988A, and fire retardant is the TDE in U.S. big lake, fire-retardant association
The antimony oxide that agent is Jinan Thailand star is imitated, composite antioxidant is antioxidant 1098 (0.25%), irgasfos 168 (0.25%).
The preparation method of above-mentioned polyamide compoiste material is identical with composite material and preparation method thereof in embodiment 3.
Polyamide compoiste material requires to carry out the detection of properties according to GB standards.
Polyamide compoiste material prepared by embodiment 1~3 and comparative example 1~2 is examined according to following examination criteria
Survey, its test result is as shown in table 1.
Table 1
Note：Melt finger test condition：230 DEG C of 2.16kg of PA6 composites；275 DEG C of 2.16kg of PA66 composites.
Claims (8)
- A kind of 1. application of multifunctional assistant in polyamide compoiste material is prepared, it is characterised in that described multifunctional assistant, It is made up of the raw material of following weight percentage：Maleic anhydride 35%-50%；Hexamethylene diamine 49.9%-64%；Antioxidant 0.05%-3%；Preparation method comprises the following steps：It is first that hexamethylene diamine and antioxidant melting mixing is uniform, the maleic anhydride of melting is then added dropwise, while during dropwise addition not Disconnected stirring, multifunctional assistant is obtained after the completion of reaction.
- 2. application of the multifunctional assistant according to claim 1 in polyamide compoiste material is prepared, it is characterised in that institute The multifunctional assistant stated, it is made up of the raw material of following weight percentage：Maleic anhydride 40%-45%；Hexamethylene diamine 54.9%-59%；Antioxidant 0.1%-1%.
- 3. application of the multifunctional assistant according to claim 1 in polyamide compoiste material is prepared, it is characterised in that with Weight, purity requirement >=99.9% of described maleic anhydride, and water content≤0.05%.
- 4. application of the multifunctional assistant according to claim 1 in polyamide compoiste material is prepared, it is characterised in that with Weight, purity requirement >=99.9% of described hexamethylene diamine, and water content≤0.05%.
- 5. application of the multifunctional assistant according to claim 1 in polyamide compoiste material is prepared, it is characterised in that institute The antioxidant stated is that antioxidant 1098, antioxidant 1010 one or both of are worked as.
- 6. application of the multifunctional assistant according to claim 1 in polyamide compoiste material is prepared, it is characterised in that institute The polyamide compoiste material stated, it is made up of the raw material of following weight percentage：Polyamide 50%-80%；Multifunctional assistant 0.1%-10%；Other components 10%-40%.
- 7. application of the multifunctional assistant according to claim 1 in polyamide compoiste material is prepared, it is characterised in that institute The multifunctional assistant stated, it is made up of the raw material of following weight percentage：
- 8. application of the multifunctional assistant according to claim 1 in polyamide compoiste material is prepared, it is characterised in that institute The polyamide compoiste material stated, it is made up of the raw material of following weight percentage：
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| DE2251821A1 (en) * | 1972-10-21 | 1974-05-02 | Basf Ag | METHOD FOR MANUFACTURING ADDITIONAL POLYMERS |
| CN101691422A (en) * | 2009-07-09 | 2010-04-07 | 重庆大学 | Preparation method for diamine polydactyl acid |
| CN103254614A (en) * | 2012-02-16 | 2013-08-21 | 合肥杰事杰新材料股份有限公司 | Bismaleimide modified thermoplastics and preparation method thereof |
-
2015
- 2015-06-15 CN CN201510329849.8A patent/CN104927085B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2251821A1 (en) * | 1972-10-21 | 1974-05-02 | Basf Ag | METHOD FOR MANUFACTURING ADDITIONAL POLYMERS |
| CN101691422A (en) * | 2009-07-09 | 2010-04-07 | 重庆大学 | Preparation method for diamine polydactyl acid |
| CN103254614A (en) * | 2012-02-16 | 2013-08-21 | 合肥杰事杰新材料股份有限公司 | Bismaleimide modified thermoplastics and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 两种双马来酰亚胺的合成与表征;武元娥等;《绝缘材料》;20140620;第47卷(第3期);第1.4节 * |
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Address after: 325011 No. 60 Gaoxi Road, hi tech park, Wenzhou economic and Technological Development Zone, Zhejiang Co-patentee after: CGN JUNER (SHANGHAI) NEW MATERIALS Co.,Ltd. Patentee after: CGN JUNER NEW MATERIALS Co.,Ltd. Address before: 325011 No. 60 Gaoxi Road, hi tech park, Wenzhou economic and Technological Development Zone, Zhejiang Co-patentee before: CGN JUNER (SHANGHAI) NEW MATERIALS Co.,Ltd. Patentee before: Zhejiang Juner New Materials Co.,Ltd. Address after: 325011 No. 60 Gaoxi Road, hi tech park, Wenzhou economic and Technological Development Zone, Zhejiang Co-patentee after: CGN JUNER (SHANGHAI) NEW MATERIALS Co.,Ltd. Patentee after: Zhejiang Juner New Materials Co.,Ltd. Address before: 325011 No. 60 Gaoxi Road, hi tech park, Wenzhou economic and Technological Development Zone, Zhejiang Co-patentee before: SHANGHAI JUNER NEW MATERIALS Co.,Ltd. Patentee before: Zhejiang Juner New Material Co.,Ltd. |