CN106749927A - A kind of preparation method of polycarbonate transparent product fire retardant - Google Patents
A kind of preparation method of polycarbonate transparent product fire retardant Download PDFInfo
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- CN106749927A CN106749927A CN201611164358.3A CN201611164358A CN106749927A CN 106749927 A CN106749927 A CN 106749927A CN 201611164358 A CN201611164358 A CN 201611164358A CN 106749927 A CN106749927 A CN 106749927A
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- fire retardant
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- transparent product
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
- C08F251/02—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof on to cellulose or derivatives thereof
-
- 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
- C08K5/16—Nitrogen-containing compounds
- C08K5/315—Compounds containing carbon-to-nitrogen triple bonds
-
- 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
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/41—Compounds containing sulfur bound to oxygen
- C08K5/42—Sulfonic acids; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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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)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a kind of preparation method of polycarbonate transparent product fire retardant：In a kettle., perfluorobutyl potassium sulfonate, perfluorobutyl ethylene, cyclodoecatriene are added by weight, (2R, 3R) 3,7, the components such as the prenylated dihydroflavonoid of 5 methoxyl group of 4' trihydroxies 8, hexadiene diphenyl silane, it is reacted to obtain product.
Description
Technical field
The present invention relates to a kind of preparation method of polycarbonate transparent product used additives, especially a kind of polycarbonate transparent
The preparation method of product fire retardant.
Background technology
Makrolon (abbreviation PC) is the high molecular polymer containing carbonate group in strand, and the three of PC engineering plastics are big
Application field is glazing, auto industry and electronics, electrical equipment industry, secondly also have industrial machinery part, CD, packaging,
The office equipments such as computer, medical and health care, film, leisure and protective equipment etc..PC can be used as door glass, PC laminates
The protective window of bank, embassy, the house of detention and public place is widely used in, for aircraft hatch cover, lighting apparatus, industry security plate washer
And bulletproof glass.
PC plate can make various labels, and such as petrol pump dial plate, fascia, warehouse and outdoor commercial signage, point type is slided
Indicator, PC resin is used for automobile lighting system, instrument panel system and built-in decoration system, as front lamp cover, band reinforcement automobile
Front and rear plate washer, reflective frame, Door frame, action bars sheath, spoiler, PC are employed to be used as terminal box, socket, plug and set
Pipe, pad, tv converter, the connector of communication cable under telephone line support, switch box, telephone exchange, distribution board unit
Part, relay1 case, PC can make low load part, device for washing one's hair, coffee machine, roasting for household electrical appliance motor, vacuum cleaner
The handle of bread producing machine, power tool, various gears, worm gear, axle sleeve, lead rule, shelf in refrigerator.PC is preferable disc storage medium
Material.
PC bottles（Container）Transparent, lightweight, impact resilience is good, and resistance to certain high temperature and etchant solution are washed, used as recyclable
Using bottle（Container）.PC and PC alloys can do computer rack, shell and subsidiary engine, printer part.Modified PC resistant to high energy radiation is killed
Bacterium, resistance to boiling and baking disinfecting, can be used for sample utensil of taking a blood sample, blood oxygenators, surgical operating instrument, kidney dialyzer etc., PC
The helmet and safety cap, protective face mask, sunglasses and motion cover glass can be made.PC films are widely used in printing chart, medical packaging,
Membrane type commutator.Fire retardant is added in makrolon manufacturing process, the fire resistance of Related product can be improved, produced
Product has security and practicality higher.
CN1313523 discloses a kind of fire retardant, it is adaptable on polyester and plastic cement.This fire retardant is to make an addition to Nano Silver
In clay, then this fire retardant is used on polyester and plastic cement, to lift its anti-flammability.The present invention is first by silver ion and clay
After being sufficiently mixed, then with reducing agent by the silver ion reduction in clay into Nano Silver.Melting when polyester master particle is manufactured is mixed
Refining state, adds Nano Silver clay that the nanometer polyester master particle of tool high fire-retardance effect is made to knead, after this nanometer of master batch is through melting,
The product for being made high flame retardant can be reprocessed.
CN104736549A discloses a kind of some phosphonates heated at a temperature of more than 200 DEG C and generates heat surely
Fire proofing that is fixed, efficient, being well suited for use as flame-retardant additive in the polymer.Fire retardant of the invention can be used
Make the unique fire retardant in a kind of composition or be used in combination with other fire retardants, synergist or adjuvant.
Fire retardant of the prior art has stronger hygroscopicity, it is impossible to is applied to damp and hot operating mode occasion, and seriously drops
The fire-retardant stability of low its addition product.When being added to polycarbonate transparent product, with makrolon poor compatibility, system can be reduced
The transparency of product.
The content of the invention
Present invention aim at above-mentioned technical problem present in solution prior art, there is provided a kind of polycarbonate transparent system
The preparation method of product fire retardant.
In order to solve the above-mentioned technical problem, the present invention is adopted the following technical scheme that：A kind of polycarbonate transparent product resistance
Fire the preparation method of agent, it is characterised in that preparation process includes：
In a kettle., 100 parts of perfluorobutyl potassium sulfonates, 1-5 parts of perfluorobutyl ethylene, 0.1-1 parts of ring are added by weight
12 carbon triolefins, 0.01-0.1 parts of (2R, 3R) -3,7,4'- trihydroxy -5- methoxyl group -8- prenylated dihydroflavonoids, 0.1-1
Part（4R-cis) -6- cyanogen methyl -2,2- dimethyl-1,3-dioxane -4- tert-butyl acetates, 1000-2000 parts of ethyl acetate,
1-5 parts of hydroxypropyl cellulose, 1-4 parts of benzoyl peroxide, reaction end obtains product.
The reaction temperature is at 80 DEG C -100 DEG C.
The reaction time 5-10h.
Described 2R, 3R) -3,7,4'- trihydroxy -5- methoxyl group -8- prenylated dihydroflavonoids be commercially available prod, such as south
The product of Jing Puyi bio tech ltd production；Perfluorobutyl potassium sulfonate is commercially available prod, the safe medicine of such as Wuhan Jiang Minhua
The product of Chemical Co., Ltd.'s production；Perfluorobutyl ethylene is commercially available prod, such as the product of Jinan Ao Chen Chemical Co., Ltd.s production
Product；（4R-cis) -6- cyanogen methyl -2,2- dimethyl-1,3-dioxane -4- tert-butyl acetates are commercially available prod, such as Chuzhou moral
The product of waffle Technology Co., Ltd. production.
Beneficial effects of the present invention：
Using perfluorobutyl potassium sulfonate used by this patent, by modification, 2R, 3R are added) -3,7,4'- trihydroxy -5- methoxies
Base -8- prenylated dihydroflavonoids,（4R-cis) -6- cyanogen methyl -2,2- dimethyl-1,3-dioxane -4- tert-butyl acetates,
Obtain flame retardant products of the invention.To the raising highly significant of the anti-flammability of polycarbonate transparent material, UL94（1.6mm）Can be with
Reach V-0 grades.
Specific embodiment
Following instance is only to further illustrate the present invention, is not limitation the scope of protection of the invention.
Embodiment 1：
In 3000L reactors, 100Kg perfluorobutyl potassium sulfonates, 3Kg perfluorobutyl ethylenes, the carbon three of 0.5Kg rings 12 are added
Alkene, 0.05Kg (2R, 3R) -3,7,4'- trihydroxy -5- methoxyl group -8- prenylated dihydroflavonoids, 0.5Kg（4R-cis) -6- cyanogen
Methyl -2,2- dimethyl-1,3-dioxane -4- tert-butyl acetates, 1500Kg ethyl acetate, 3Kg hydroxypropyl celluloses, 2Kg
Benzoyl peroxide, reacts 8h under the conditions of 90 DEG C, and reaction end obtains product.Production code member M-1.
Embodiment 2：
In 3000L reactors, 100Kg perfluorobutyl potassium sulfonates, 1Kg perfluorobutyl ethylenes, the carbon three of 0.1Kg rings 12 are added
Alkene, 0.01Kg (2R, 3R) -3,7,4'- trihydroxy -5- methoxyl group -8- prenylated dihydroflavonoids, 0.1Kg（4R-cis) -6- cyanogen
Methyl -2,2- dimethyl-1,3-dioxane -4- tert-butyl acetates, 1000Kg ethyl acetate, 1Kg hydroxypropyl celluloses, 1Kg
Benzoyl peroxide, reacts 5h under the conditions of 80 DEG C, and reaction end obtains product.Production code member M-2.
Embodiment 3：
In 3000L reactors, addition 100Kg perfluorobutyl potassium sulfonates, 5Kg perfluorobutyl ethylenes, 1Kg cyclodoecatrienes,
0.1Kg (2R, 3R) -3,7,4'- trihydroxy -5- methoxyl group -8- prenylated dihydroflavonoids, 1Kg（4R-cis) -6- cyanogen methyl -
2,2- dimethyl-1,3-dioxane -4- tert-butyl acetates, 2000Kg ethyl acetate, 5Kg hydroxypropyl celluloses, 4Kg peroxidating
Benzoyl, reacts 10h under the conditions of 100 DEG C, and reaction end obtains product.Production code member M-3.
Comparative example 1：Cyclodoecatriene is added without, the other the same as in Example 1.Products obtained therefrom numbering is M-4.
Comparative example 2：(2R, 3R) -3,7,4'- trihydroxy -5- methoxyl group -8- prenylated dihydroflavonoids are added without, other
With embodiment 1.Products obtained therefrom numbering is M-5.
Comparative example 3：（4R-cis) -6- cyanogen methyl -2,2- dimethyl-1,3-dioxane -4- tert-butyl acetates are added without,
The other the same as in Example 1.Products obtained therefrom numbering is M-6.
Embodiment 4：
The fire retardant dosage 0.05wt% of embodiment 1-3 and comparative example 1-3 will be added, be applied to the combination of polycarbonate transparent material
In thing, fire resistance is detected by ANST/UL94-1985.
Light transmittance is detected by JG-T116-1999.
The comparing of the test specimen fire resistance that the different process of table 1 is made
| Numbering | Fire resistance UL94（1.6mm） | Light transmittance % |
| M-1 | V-0 | 87 |
| M-2 | V-0 | 87 |
| M-3 | V-0 | 88 |
| M-4 | V-1 | 85 |
| M-5 | V-1 | 85 |
| M-6 | V-1 | 84 |
| It is not added with flame retardant polycarbonate | V-1 | 88 |
As shown in Table 1：Fire retardant dosage 0.05wt%, to the raising highly significant of the anti-flammability of polycarbonate transparent material, UL94
（1.6mm）V-0 grades can be reached, while the transparency of polycarbonate article is not reduced.
Claims (3)
1. a kind of preparation method of polycarbonate transparent product fire retardant, it is characterised in that comprise the following steps：
In a kettle., 100 parts of perfluorobutyl potassium sulfonates, 1-5 parts of perfluorobutyl ethylene, 0.1-1 parts of ring are added by weight
12 carbon triolefins, 0.01-0.1 parts of (2R, 3R) -3,7,4'- trihydroxy -5- methoxyl group -8- prenylated dihydroflavonoids, 0.1-1
Part（4R-cis) -6- cyanogen methyl -2,2- dimethyl-1,3-dioxane -4- tert-butyl acetates, 1000-2000 parts of acetic acid second
Ester, 1-5 parts of hydroxymethyl cellulose, 1-4 parts of benzoyl peroxide, reaction end obtains product.
2. the preparation method of a kind of polycarbonate transparent product fire retardant described in claim 1, it is characterised in that：It is described anti-
Temperature is answered at 80 DEG C -100 DEG C.
3. the preparation method of a kind of polycarbonate transparent product fire retardant described in claim 1, it is characterised in that：It is described anti-
5-10h between seasonable.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611164358.3A CN106749927A (en) | 2016-12-16 | 2016-12-16 | A kind of preparation method of polycarbonate transparent product fire retardant |
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| CN201611164358.3A CN106749927A (en) | 2016-12-16 | 2016-12-16 | A kind of preparation method of polycarbonate transparent product fire retardant |
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| CN201611164358.3A Pending CN106749927A (en) | 2016-12-16 | 2016-12-16 | A kind of preparation method of polycarbonate transparent product fire retardant |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4043980A (en) * | 1976-05-18 | 1977-08-23 | Mobay Chemical Corporation | Flame retardant polycarbonate having improved critical thickness |
| CN101497742A (en) * | 2009-03-09 | 2009-08-05 | 佛山市顺德区瑞能科技有限公司 | Halogen-free flame-retardant composition and use thereof |
-
2016
- 2016-12-16 CN CN201611164358.3A patent/CN106749927A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4043980A (en) * | 1976-05-18 | 1977-08-23 | Mobay Chemical Corporation | Flame retardant polycarbonate having improved critical thickness |
| CN101497742A (en) * | 2009-03-09 | 2009-08-05 | 佛山市顺德区瑞能科技有限公司 | Halogen-free flame-retardant composition and use thereof |
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Effective date of registration: 20180822 Address after: 200433 C149 64, 1426 military industrial road, Yangpu District, Shanghai. Applicant after: Shanghai Pu Xin polymer materials Co., Ltd. Address before: 324000 8-1 Donggang eight road, Kecheng District, Quzhou, Zhejiang Applicant before: Quzhou universal New Material Co., Ltd. |
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Application publication date: 20170531 |