CN104292525A - Flame retardant rubber and preparation method thereof - Google Patents
Flame retardant rubber and preparation method thereof Download PDFInfo
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- CN104292525A CN104292525A CN201410604313.8A CN201410604313A CN104292525A CN 104292525 A CN104292525 A CN 104292525A CN 201410604313 A CN201410604313 A CN 201410604313A CN 104292525 A CN104292525 A CN 104292525A
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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
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/58—Component parts, details or accessories; Auxiliary operations
- B29B7/72—Measuring, controlling or regulating
- B29B7/726—Measuring properties of mixture, e.g. temperature or density
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/58—Component parts, details or accessories; Auxiliary operations
- B29B7/72—Measuring, controlling or regulating
- B29B7/728—Measuring data of the driving system, e.g. torque, speed, power, vibration
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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Abstract
The invention relates to flame retardant rubber and a preparation method thereof. The flame retardant rubber is prepared from the following raw materials in parts by weight: 100 parts of natural rubber matrix, 2-4 parts of vulcanizing agents, 2-4 parts of accelerants, 1-10 part of a fire retardant, 2-6 parts of processing agents and 3-5 parts of anti-aging agents. According to the invention, compared with the prior art, the center temperature of the thermal weight loss of the flame retardant rubber is 396.3 DEG C, and the burning rate is 19.48 mm/min, so that dendriform organic montmorillonite can be modified into natural rubber, the flame retardant and natural rubber with good inflaming retarding performance, thermal stability performance and mechanical performance can be obtained, and montmorillonite can be stripped controllably and dispersed uniformly in a polymer matrix, and has good compatibility with a polymer.
Description
Technical field
The invention belongs to technical field of rubber material, especially relate to a kind of flame retardant rubber and preparation method thereof.
Background technology
The natural high moleculer eompound of natural rubber to be a kind of with polyisoprene be main component, molecular formula is (C5H8) n, in its composition, 91% ~ 94% is rubber hydrocarbon (polyisoprene), and all the other are the nonrubber materials such as protein, lipid acid, ash content, carbohydrate.Natural rubber is most widely used conventional rubber.Natural rubber, as general elastomeric material, is widely used in automobile, plane tyre, adhesive tape, sebific duct, water-proof material, and rubber overshoes, gloves, electrical accessorie etc., and the life of people is closely bound up.But general natural rubber oxygen index is about 17%, and easily burn, and can discharge a large amount of black smoke in combustion, therefore fire-retardant the and thermal stability of natural rubber is extremely important.
Traditional halogen fire retardant can reach good flame retardant effect, but it can discharge poisonous hydrogen halide in combustion, works the mischief to human body, environment; And inorganic fire-retarded filler often needs very high addition could meet flame-retardancy requirements, but affect the use properties of material.The fire-retardant fire retardant mostly still adopted containing halogen of current natural rubber, along with people are to environmental protection and the raising to material performance requirement, develops the focus that novel effective, eco-friendly fire retardant systems has become research.
In recent years, along with people are to the further investigation of nanotechnology, utilize some special effectses of the size of nanometer fire-retardant to realize, cause the attention of people.Nano-meter flame retardants, generally comprises nano-powder and the large class of layered silicate two.Nano-powder is mainly nano-sized magnesium hydroxide, nano-aluminum hydroxide etc., but their addition generally all will reach more than 30 parts just shows good flame retardant effect.And the organic layered silicate salt/polymer nanocomposites utilizing intercalation technique to prepare is compared with traditional filled polymer, the mechanical property of polymeric matrix, gas barrier property and solvent resistance can not only be improved, also there is potential flame retardant resistance and burn from putting out the features such as feature.
Result of study shows, the dendriform organo montmorillonite price that both alternative or Some substitute was traditional is higher, environment is unfriendly and the fire-retardant and supporting material of other performance of infringement polymkeric substance, as: halogen flame, expansion type flame retardant, hydroxide flame retardant, white carbon black and carbon black etc., can improve again the performances such as the fire-retardant of elastomeric material and mechanics.But how to use dendriform organo montmorillonite to carry out modification to natural rubber, realize the controlled stripping of polynite and the dispersed and consistency in polymeric matrix thereof, obtain the Flame-retardant natural rubber that flame retardant effect, thermostability and mechanical property are all excellent, relevant report that so far there are no.
Chinese patent CN101792544 discloses environment-friendly flame retardant rubber material and preparation method thereof, its component comprises rubber matrix, vulcanizing agent, promotor, stearic acid, zinc oxide, anti-aging agent, fire retardant etc., the flame retardant rubber good flame retardation effect prepared, mechanical property and wear resisting property relative good.What above-mentioned fire retardant was chosen is quaternary ammonium salt and polynite react make organo montmorillonite, its mechanical property and flame retardant effect are comparatively worse than the dendriform montmorillonite flame-retardant agent in this patent.
Summary of the invention
Object of the present invention be exactly in order to overcome above-mentioned prior art exist defect and a kind of application requiring meeting natural rubber is provided.
Object of the present invention can be achieved through the following technical solutions:
A kind of flame retardant rubber, is prepared by the raw material of following component and weight part content:
Natural rubber matrix 100; Vulcanizing agent 2 ~ 4; Promotor 2 ~ 4; Fire retardant 1 ~ 10; Processing aid 2 ~ 6; Anti-aging agent 3 ~ 5.
Described fire retardant is dendriform organo montmorillonite, this organo montmorillonite take hexachlorocyclotriphosphazene as core by the Michael reaction of quadrol and methyl acrylate, the dendritic polymer of synthesis containing phosphorus nitrogen, and undertaken organically-modified by MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, synthesis organo montmorillonite, finally carries out modification to the Amino End Group synthesizing the dendritic polymer obtained.
Sodium methylate is added as catalyzer in described Michael reaction.
Described vulcanizing agent is sulphur.
Described promotor is 2-benzothiazolyl mercaptan and Sodium dimethyldithiocarbamate 40min is 2: 1 ~ 6: 1 compound formed in mass ratio.
Described processing aid is stearic acid and zinc oxide 1: 3 ~ 3: 1 compound formed in mass ratio.
Described anti-aging agent is N-sec.-propyl-N '-diphenyl-para-phenylene diamine.
The preparation method of flame retardant rubber adopts following steps:
A) regulate the roller temperature of rubber mixing mill between 30 ~ 60 DEG C, natural rubber matrix, promotor, processing aid and anti-aging agent are dropped in mill carry out mixing 20 ~ 30min successively;
B) adjust the roll spacing of mill to 0.5 ~ 1.5mm, add fire retardant, smash glue, mixing 5 ~ 15min;
C) adjust the roll spacing of mill again to 3 ~ 5mm, continue mixing 10 ~ 20min, until form the sizing material of smooth zero-clearance;
D) by step c) gained sizing material roll-in slice, after film at room temperature naturally cooling, again drops in mill, adds vulcanizing agent, carry out discharging, sulfuration, prepare flame retardant rubber.
The present invention adopts dendriform polynite as fire retardant, mainly there is the hexachlorocyclotriphosphazene of higher thermal temperature performance for core with phosphorous, nitrogen, the dendritic flame-retardant polymkeric substance of 24 arm ends is synthesized by the Michael addition of methyl acrylate that replaces and the amidate action of quadrol, and react with the organo montmorillonite after quaternary ammonium salt-MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (DMC) intercalation with high thermal stability, final dendritic flame-retardant polynite.The final residual volume of this dendritic flame-retardant polynite is 61%, and thermal weight loss core temperature is 200.2 DEG C.And the dendritic flame-retardant polynite in Zhao Yi master thesis carries out organic modification by Tetrakis hydroxymethyl phosphonium chloride (THPC) to sodium-based montmorillonite, modified organo montmorillonite and AB
2intermediate (diethanolamine and methyl acrylate generation Michael reaction, thus prepare end group and contain hydroxyl, and there is the compound of ester group one end) step reaction, final dendritic flame-retardant polynite.Because the thermal stability of this intermediate is lower, so the thermal stability of dendritic flame-retardant polynite is lower.
Compared with prior art, the thermal weight loss core temperature of the flame retardant rubber that the present invention prepares is 396.3 DEG C, rate of combustion is 19.48mm*min, achieve with the organic imvite modified natural rubber of dendriform, obtain the Flame-retardant natural rubber that the performances such as fire-retardant, thermally-stabilised and mechanics are all excellent, and the controlled stripping of polynite achieved wherein and dispersed in polymeric matrix thereof and the excellent compatibility with polymkeric substance, and use safety environmental protection, there is potential economic benefit and social effect.
Embodiment
Below in conjunction with embodiment and comparative example, technical scheme of the present invention is described in further detail and completely.Organo montmorillonite described in embodiment and dendriform organo montmorillonite are all adopt following methods to prepare: the inorganic polynite of 20g adds in deionized water, is mixed with the suspension that massfraction is 5%; Gained suspension is placed in the water bath with thermostatic control of 60 DEG C, 30g MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride is added in suspension, finishes, insulation reaction 5h under violent stirring, filters, with deionized water wash filter cake to existing without Cl-, 80 DEG C of oven dry, obtain the organo montmorillonite of modification.In flask, add 2.5g massfraction is that the G-1 of 20% is for the methanol aqueous solution of Amino End Group polyamidoamine Triphosphazene dendritic macromole; under N2 protection; the organo montmorillonite 10g that modification obtains slowly is added at 50 DEG C; finish; insulation reaction 7h under violent stirring; filter, dry pale powder solid, be high heat-resisting, the high fire retardant pressing down cigarette.Embodiment is tested the physical and mechanical properties of obtained flame-retardant natural rubber and flame retardant properties with reference to GB 528-83 and GB/T10707 standard.Adopt the thermogravimetry that " nano composite polymer/laminated silicate material theory and practice " (QiZongNeng, Shang Wenyu writes, Chemical Industry Press, 2002) specifies, the thermal weight loss core temperature of test Flame-retardant natural rubber, T
max.
Embodiment 1
Regulate the roller temperature of rubber mixing mill to 30 DEG C, successively 100g natural rubber matrix, 2g captax, 0.5g promotor S, 1g stearic acid, 1g zinc oxide, 3g antioxidant 4010 A are dropped in mill, mixing 20min;
Adjustment roll spacing, to 0.5mm, adds 1g dendriform organo montmorillonite, smashes glue, mixing 5min; Adjust roll spacing again to 3mm, continue mixing about 10min, until form the glue-line of smooth zero-clearance;
By gained sizing material roll-in slice, treat film at room temperature naturally cooling 8h, again drop in mill, add 2g sulphur, carry out discharging, sulfuration, obtain described Flame-retardant natural rubber.
The tensile strength of gained natural rubber, elongation at break, horizontal burn rate and thermal weight loss core temperature (T
max) test data in table 1.
Comparative example 1
By 100g natural rubber, 2g sulphur, 2g captax, 0.5g promotor S, 1g organo montmorillonite, 1g stearic acid, 1g zinc oxide and 3g antioxidant 4010NA, drop in mill, evenly mixing at 30 DEG C, obtain common natural rubber.
The tensile strength of common natural rubber, elongation at break, horizontal burn rate and thermal weight loss core temperature (T
max) test data in table 1.
Embodiment 2
Regulate the roller temperature of rubber mixing mill to 45 DEG C, successively by 100g natural rubber, 2.5g captax, 0.7g promotor S, 2g stearic acid, 2g zinc oxide, 4g antioxidant 4010NA, drop in mill, mixing 25min;
Adjustment roll spacing, to 1mm, adds 5g dendriform organo montmorillonite, smashes glue, mixing 10min; Adjust roll spacing again to 4mm, continue mixing 15min, until form the glue-line of smooth zero-clearance;
By gained sizing material roll-in slice, treat film at room temperature naturally cooling 16h, again drop in mill, add 3g sulphur, carry out discharging, sulfuration, obtain described Flame-retardant natural rubber.
The tensile strength of gained natural rubber, elongation at break, horizontal burn rate and thermal weight loss core temperature (T
max) test data in table 1.
Comparative example 2
100g natural rubber, 3g sulphur, 2.5g captax, 0.7g promotor S, 5g organo montmorillonite, 2g stearic acid, 2g zinc oxide and 4g antioxidant 4010NA are dropped in mill, evenly mixing at 45 DEG C, obtain common natural rubber.
The tensile strength of common natural rubber, elongation at break, horizontal burn rate and thermal weight loss core temperature (T
max) test data in table 1.
Embodiment 3
Regulate the roller temperature of rubber mixing mill to 60 DEG C, successively by 100g natural rubber, 3g captax, 0.9g promotor S, 3g stearic acid, 3g zinc oxide, 5g antioxidant 4010NA, drop in mill, mixing 30min;
Adjustment roll spacing, to 1.5mm, adds 10g dendriform organo montmorillonite, smashes glue, mixing 15min; Adjust roll spacing again to 5mm, continue mixing 20min, until form the glue-line of smooth zero-clearance;
By gained sizing material roll-in slice, treat film at room temperature naturally cooling 24h, again drop in mill, add 4g sulphur, carry out discharging, sulfuration, obtain described Flame-retardant natural rubber.
The tensile strength of gained natural rubber, elongation at break, horizontal burn rate and thermal weight loss core temperature (T
max) test data in table 1.
Comparative example 3
100g natural rubber, 4g sulphur, 3g captax, 0.9g promotor S, 10g organo montmorillonite, 3g stearic acid, 3g zinc oxide and 5g antioxidant 4010NA are dropped in mill, evenly mixing at 60 DEG C, obtain common natural rubber.
The tensile strength of common natural rubber, elongation at break, horizontal burn rate and thermal weight loss core temperature (T
max) test data in table 1.
Table 1
Can be shown by the test result of table 1: present invention achieves with the organic imvite modified natural rubber of dendriform, obtain fire-retardant, that the performance such as thermostability and mechanics is all excellent Flame-retardant natural rubber, and the controlled stripping of polynite achieved wherein and dispersed in polymeric matrix thereof and the excellent compatibility with polymkeric substance, significantly improve the smoke suppressing effect of natural gum.Visible, dendriform organo montmorillonite/natural rubber nano composite material a kind of novelly has flame-retarded efficiency and eco-friendly fire retardant material.
Finally be necessary described herein: above embodiment is only for being described in more detail technical scheme of the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.
Claims (10)
1. a flame retardant rubber, is characterized in that, is prepared by the raw material of following component and weight part content:
Natural rubber matrix 100; Vulcanizing agent 2 ~ 4; Promotor 2 ~ 4; Fire retardant 1 ~ 10; Processing aid 2 ~ 6; Anti-aging agent 3 ~ 5.
2. a kind of flame retardant rubber according to claim 1, it is characterized in that, described fire retardant is dendriform organo montmorillonite, this organo montmorillonite take hexachlorocyclotriphosphazene as core by the Michael reaction of quadrol and methyl acrylate, the dendritic polymer of synthesis containing phosphorus nitrogen, and being undertaken organically-modified by MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, synthesis organo montmorillonite, finally carries out modification to the Amino End Group synthesizing the dendritic polymer obtained.
3. a kind of flame retardant rubber according to claim 2, is characterized in that, adds sodium methylate as catalyzer in described Michael reaction.
4. a kind of flame retardant rubber according to claim 1, is characterized in that, described vulcanizing agent is sulphur.
5. a kind of flame retardant rubber according to claim 1, is characterized in that, described promotor is 2-benzothiazolyl mercaptan and Sodium dimethyldithiocarbamate 40min is 2: 1 ~ 6: 1 compound formed in mass ratio.
6. a kind of flame retardant rubber according to claim 1, is characterized in that, described processing aid is stearic acid and zinc oxide 1: 3 ~ 3: 1 compound formed in mass ratio.
7. a kind of flame retardant rubber according to claim 1, is characterized in that, described anti-aging agent is N-sec.-propyl-N '-diphenyl-para-phenylene diamine.
8. the preparation method of the flame retardant rubber according to any one of claim 1-7, is characterized in that, adopts following steps:
A) regulate the roller temperature of rubber mixing mill between 30 ~ 60 DEG C, evenly mixing by carrying out in natural rubber matrix, promotor, processing aid and the mill of anti-aging agent input successively;
B) adjust the roll spacing of mill to 0.5 ~ 1.5mm, add fire retardant, smash glue, mixing 5 ~ 15min;
C) adjust the roll spacing of mill again to 3 ~ 5mm, continue mixing, until form the sizing material of smooth zero-clearance;
D) by step c) gained sizing material roll-in slice, after film at room temperature naturally cooling, again drops in mill, adds vulcanizing agent, carry out discharging, sulfuration, prepare flame retardant rubber.
9. the preparation method of a kind of flame retardant rubber according to claim 8, is characterized in that, step a) middle mixing time is 20 ~ 30min.
10. the preparation method of a kind of flame retardant rubber according to claim 8, is characterized in that, step c) in mixing time be 10 ~ 20min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104710652A (en) * | 2015-03-27 | 2015-06-17 | 上海工程技术大学 | Dendritic modified montmorillonite flame retardant and preparation method thereof |
| CN104710657A (en) * | 2015-03-27 | 2015-06-17 | 上海工程技术大学 | Flame-retardant rubber and preparation method thereof |
| CN111202288A (en) * | 2020-02-20 | 2020-05-29 | 云南电网有限责任公司电力科学研究院 | Method for manufacturing low-pressure protection labor protection gloves |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104710652A (en) * | 2015-03-27 | 2015-06-17 | 上海工程技术大学 | Dendritic modified montmorillonite flame retardant and preparation method thereof |
| CN104710657A (en) * | 2015-03-27 | 2015-06-17 | 上海工程技术大学 | Flame-retardant rubber and preparation method thereof |
| CN111202288A (en) * | 2020-02-20 | 2020-05-29 | 云南电网有限责任公司电力科学研究院 | Method for manufacturing low-pressure protection labor protection gloves |
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| CN104292525B (en) | 2016-04-27 |
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