CN103408743B - Can directly spin production method and the system of copolymerization Phosphorous Flame-Retardant Polyester by continuous seepage - Google Patents
Can directly spin production method and the system of copolymerization Phosphorous Flame-Retardant Polyester by continuous seepage Download PDFInfo
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Abstract
The present invention relates to and a kind ofly can directly spin production method and the system of copoly type Phosphorous Flame-Retardant Polyester by continuous seepage, adopt continuous condensed Pet Production Line, at least comprise first, second esterifier be connected successively, described method prepares fire retardant pre-esterification liquid for adopting phosphorus flame retardant and ethylene glycol by semi-continuous process, then described fire retardant pre-esterification liquid is injected described second esterifier continuously, described system comprises the pre-esterification reactor device for the preparation of fire retardant pre-esterification liquid, and the outlet of described pre-esterification reactor device connects described second esterifier by pipeline.The present invention is under the processing parameter and specific device structure condition of uniqueness, and in the flame retardant polyester of production, ignition-proof element content is high, and associativity is good, and product performance are stablized, and flexibility of operation is strong, product anti-dropping.
Description
Technical field
The present invention relates to a kind of production method and system of polyester, particularly relate to and a kind ofly can directly spin production method and the system of copolymerization Phosphorous Flame-Retardant Polyester by continuous seepage.
Background technology
Flame retardant polyester is important functional polyester, and along with the issuing and implementation about laws and rules such as fire-fightings, demand will sharply increase.The preparation method of flame retardant polyester mainly contains blended, copolymerization and Final finishing etc., along with the development of reactive flame retardant, the advantages such as modification by copolymerization is obvious with flame retardant effect, good endurance become the predominant methods preparing flame retardant polyester gradually, and phosphorous copoly type flame retardant polyester, because its permanent, low cigarette, hypotoxicity will be widely used in numerous areas.
But at present both at home and abroad continuous industrial production is little, substantially based on the technical process of batchwise polymerization or semi-continuous polymerzation, throughput is little, starting material and energy expenditure large, product cost is high, unstable product quality.
Current domestic disclosed fire retardant co-polymerization modified polyester production method mainly divides two kinds, the first is the esterifying liquid adding fire retardant 2-carboxyethyl phenyl Hypophosporous Acid, 50 and ethylene glycol in polycondensation phase, this can cause flame retardant agent content in flame retardant polyester segment lower, and adverse influence can be produced to polycondensation vacuum system, be unfavorable for device continuous and stable production.The second is directly joined by fire retardant in esterification mixed slurry, follow-up normal polyester Production Flow Chart, and this technique is comparatively simple, but its ignition-proof element skewness in final polyester segment, and associativity is poor.
Summary of the invention
For overcoming the above-mentioned defect of prior art, the object of the present invention is to provide and a kind ofly can directly spin production method and the system of copoly type Phosphorous Flame-Retardant Polyester by continuous seepage, the flame retardant polyester of high flame retardant constituent content can be produced, and ignition-proof element associativity is good, stable performance, flexibility of operation is strong.
The technical solution used in the present invention is: a kind ofly can directly spin the production method of copoly type Phosphorous Flame-Retardant Polyester by continuous seepage, adopt continuous condensed Pet Production Line, at least comprise the first esterifier and the second esterifier that are connected successively, adopt phosphorus flame retardant and ethylene glycol to carry out pre-esterification by semi-continuous process and prepare fire retardant pre-esterification liquid, described fire retardant pre-esterification liquid is injected described second esterifier continuously.
The acid value of described fire retardant pre-esterification liquid is preferably 95 ~ 125mgKOH/g.
In described fire retardant pre-esterification liquid, the mass content of phosphoric is preferably not less than 3.5%.
The mass ratio of described phosphorus flame retardant and ethylene glycol can be 1:2.20 ~ 1:1.05, and in the process of pre-esterification, working pressure scope can be 5 ~ 20kPa(G), operating temperature range can be 110 ~ 220 DEG C, and reaction time can be 1 ~ 3h.
Preferably, described second esterifier is horizontal esterifier, and its inner chamber is divided into the first chamber, the second chamber and the 3rd chamber from left to right, is equipped with whipping appts in each chamber, and described fire retardant pre-esterification liquid injects described second chamber.
Working pressure scope in described second esterifier can be 0 ~ 20kPa(G), operating temperature range in described first, second, and third chamber can be followed successively by 240 ~ 255 DEG C, 230 ~ 245 DEG C and 250 ~ 265 DEG C, and the reaction time in described first, second, and third chamber can be followed successively by 15 ~ 30min, 20 ~ 40min and 30 ~ 50min.
A kind of adopt aforesaid method can directly spin the production system of copoly type Phosphorous Flame-Retardant Polyester by continuous seepage, comprise continuous condensed Pet Production Line, described continuous condensed Pet Production Line at least comprises the first esterifier and the second esterifier that are connected successively, also comprise the pre-esterification reactor device for the preparation of fire retardant pre-esterification liquid, the outlet of described pre-esterification reactor device connects described second esterifier by pipeline.
Pipeline between the outlet of described pre-esterification reactor device and the second esterifier can be connected with fire retardant pre-esterification liquid charging tank, the pipeline between described fire retardant pre-esterification liquid charging tank and the second esterifier can be provided with charging pump.
Preferably, described second esterifier is horizontal esterifier, its inner chamber is divided into the first chamber, the second chamber and the 3rd chamber from left to right, is equipped with whipping appts in each chamber, and the outlet of described pre-esterification reactor device connects described second chamber by described pipeline.
Described first chamber can be connected additive material source respectively by corresponding pipeline with the 3rd chamber.
Beneficial effect of the present invention: under the processing parameter and specific device structure condition of uniqueness of the present invention, in the flame retardant polyester produced, phosphorus element content is high and associativity good, mass content can reach 0.5 ~ 1.2%, limiting oxygen index(LOI) is not less than 28%, fusing point is not less than 245 DEG C, and viscosity fluctuation range-controllable is built in ± 0.01dl/g, and product performance are stablized, flexibility of operation is strong, anti-dropping.
Pre-esterification prepares the processing condition of the uniqueness that fire retardant pre-esterification liquid adopts, make fire retardant stability high, esterification fully and side reaction can be inhibited, reaction system can realize liquid homogeneous reaction, in the fire retardant pre-esterification liquid obtained, ignition-proof element is evenly distributed and stability is high, be conducive to further esterification and polycondensation production flame retardant polyester product, combine with follow-up esterification technique condition, achieve the optimization of each composition and each reactions steps in esterification technique, be not only the continuous seepage of flame retardant polyester thus and directly spin the condition of providing, but also be conducive to improving effective phosphorus content and flame retardant properties in product.
Fire retardant pre-esterification liquid injects the second chamber of the low temperature of the second esterifier and controls cooperatively interacting of second esterifier three chamber temps, while guarantee esterification is carried out smoothly, be beneficial to the stability keeping low-temperature flame retardant agent pre-esterification liquid at addition point on the one hand, on the other hand be beneficial to the fire retardant pre-esterification liquid esterification polymer segment association reaction close with its homogeneity thus reach ignition-proof element being uniformly distributed in the product, overcome ignition-proof element under prior art skewness and the poor defect of associativity in final polyester segment thus, flame retardant properties is significantly improved, and ensure that carrying out smoothly of actual process process, because the fire retardant in this patent is high in synthetic system interior heat stability, strong with polymer segment associativity, variable middle polymer is not generated in reaction process, therefore in production process without the need to adding thermo-stabilizer, other auxiliary agent such as antioxidant.
Accompanying drawing explanation
Fig. 1 is the simple process schematic diagram of system of the present invention;
Fig. 2 is the structural representation of a kind of embodiment of system of the present invention.
Embodiment
The invention provides and a kind ofly can directly spin the production method of copoly type Phosphorous Flame-Retardant Polyester by continuous seepage, realize based on continuous condensed Pet Production Line, described continuous condensed Pet Production Line, at least comprise the first esterifier and the second esterifier that are connected successively, the method employing phosphorus flame retardant and ethylene glycol carry out pre-esterification by semi-continuous process and prepare fire retardant pre-esterification liquid, then the described fire retardant pre-esterification liquid of preparation are injected described second esterifier continuously.The method technological process is simple, and production efficiency and high efficiency, production cost is low, constant product quality.
The acid value of described fire retardant pre-esterification liquid is preferably 95 ~ 125mgKOH/g, and as 95mgKOH/g, 100mgKOH/g, 110mgKOH/g, 120mgKOH/g or 125mgKOH/g, wherein the mass content of phosphoric is preferably not less than 3.5%.At this point in the reaction, fire retardant stability is high, esterification fully and side reaction be inhibited, reaction system can realize liquid homogeneous reaction, in the fire retardant pre-esterification liquid obtained, ignition-proof element is evenly distributed and stability is high, is conducive to further esterification and flame retardant polyester product is produced in polycondensation.
When preparing described fire retardant pre-esterification liquid, pre-esterification degree can be controlled by regulating the reactant formula in pre-esterification process, temperature, pressure and reaction times, preferably, the mass ratio of described phosphorus flame retardant and ethylene glycol is 1:2.20 ~ 1:1.05, as: 1:2.20,1:2.00,1:1.75,1:1.20 or 1:1.05; In the process of pre-esterification, working pressure scope is 5 ~ 20kPa(G), as 5kPa(G), 10kPa(G), 15kPa(G), 18kPa(G) or 20kPa(G); Operating temperature range is 110 ~ 220 DEG C, as 110 DEG C, 150 DEG C, 180 DEG C, 200 DEG C or 220 DEG C; Reaction time is 1 ~ 3h, as 1h, 1.5h, 2h, 2.5h or 3h.
Preferably, described second esterifier is horizontal esterifier, and its inner chamber is divided into the first chamber, the second chamber and the 3rd chamber from left to right, is equipped with whipping appts in each chamber, and described fire retardant pre-esterification liquid injects described second chamber.Working pressure scope in described second esterifier can be 0 ~ 20kPa(G), as 0kPa(G), 5kPa(G), 10kPa(G), 15kPa(G) or 20kPa(G), operating temperature range in described first chamber can be 240 ~ 255 DEG C, as 240 DEG C, 245 DEG C, 250 DEG C or 255 DEG C, reaction time can be 15 ~ 30min, as 15min, 20min, 25min or 30min; Operating temperature range in described second chamber can be 230 ~ 245 DEG C, and as 230 DEG C, 235 DEG C, 240 DEG C or 245 DEG C, reaction time can be 20 ~ 40min, as 20min, 25min, 30min, 35min or 40min; Operating temperature range in described 3rd chamber can be 250 ~ 265 DEG C, and as 250 DEG C, 255 DEG C, 260 DEG C or 265 DEG C, reaction time can be 30 ~ 50min, as 30min, 35min, 40min, 45min or 50min.
Described fire retardant pre-esterification liquid is added to the second chamber of the low temperature of described second esterifier and controls cooperatively interacting of described second esterifier three chamber temps, while guarantee esterification is carried out smoothly, be beneficial on the one hand the stability keeping low-temperature flame retardant agent pre-esterification liquid at addition point, be beneficial to the fire retardant pre-esterification liquid esterification polymer segment association reaction close with its homogeneity on the other hand thus reach ignition-proof element being uniformly distributed in the product.
Method of the present invention is under the processing parameter and specific device structure condition of above-mentioned uniqueness, in the flame retardant polyester produced, phosphorus element content is high and associativity good, mass content can reach 0.5 ~ 1.2%, limiting oxygen index(LOI) is not less than 28%, fusing point is not less than 245 DEG C, and viscosity fluctuation range-controllable is built in ± 0.01dl/g, and product performance are stablized, flexibility of operation is strong, anti-dropping.
See Fig. 1 and Fig. 2, present invention also offers a kind of adopt aforesaid method can directly spin the production system of copoly type Phosphorous Flame-Retardant Polyester by continuous seepage, comprise continuous condensed Pet Production Line, described continuous condensed Pet Production Line at least comprises the first esterifier 1 and the second esterifier 2 be connected successively, also comprise the pre-esterification reactor device 3 for the preparation of fire retardant pre-esterification liquid, the outlet of described pre-esterification reactor device connects described second esterifier by pipeline, for the fire retardant pre-esterification liquid of preparation is injected described second esterifier continuously, certainly, other esterifier can also be added in actual applications as required to realize more multistep esterification.
Before described first esterifier, slurry preparation groove 4 can be set, during production, raw material PTA and EG is mixed and made into suspension by process ratio metering, the polycondensation catalyst ethylene glycol solution prepared is metered into described slurry preparation groove from catalyzer charging tank simultaneously, described first esterifier is quantitatively sent into by spiral pump through well-mixed PTA, EG and catalyst mixture slurry, in addition, can add the additive of other purposes by needs of production, these adjustment can realize according to existing and other correlation techniques.
The slurry sending into described first esterifier fully reacts and reaches more than 90% to esterification yield under certain temperature, pressure, liquid level, is then sent to described second esterifier.Preferably, described second esterifier is horizontal esterifier, outside is provided with heating agent chuck, its inner chamber is divided into the first chamber 5, second chamber 6 and the 3rd chamber 7 from left to right, whipping appts is equipped with in each chamber, what the top of described second chamber was provided with described fire retardant pre-esterification liquid adds entrance, what the outlet of described pre-esterification reactor device connected the described fire retardant pre-esterification liquid of described second chamber by described pipeline adds entrance, so that described fire retardant pre-esterification liquid is injected described second chamber.Material in three chambers of described second esterifier at different temperature and level conditions after abundant stirring reaction (esterification yield is not less than 98%) be sent to subsequent technique, after the process of subsequent technique, be prepared into flame retardant polyester product.
Described pre-esterification reactor device can adopt vertical fully mixing reactor, and is provided with knockout tower 8 with the water produced in separating reaction and the ethylene glycol evaporated in condensation reaction.Pipeline between the outlet of described pre-esterification reactor device and the second esterifier (the adding entrance of fire retardant pre-esterification liquid) can be connected with fire retardant pre-esterification liquid charging tank 9, stand-by for storing the described fire retardant pre-esterification liquid prepared, pipeline between described fire retardant pre-esterification liquid charging tank and the second esterifier can be provided with charging pump, and the fire retardant pre-esterification liquid be stored in described fire retardant pre-esterification liquid charging tank can inject continuously in the second chamber of described second esterifier via described charging pump after accurate measurement.
The top of described first chamber and the 3rd chamber can be respectively equipped with additive and add entrance, and connects additive material source respectively by corresponding pipeline.
Claims (7)
1. one kind can directly be spun the production method of copoly type Phosphorous Flame-Retardant Polyester by continuous seepage, adopt continuous condensed Pet Production Line, at least comprise the first esterifier and the second esterifier that are connected successively, it is characterized in that adopting phosphorus flame retardant and ethylene glycol to carry out pre-esterification by semi-continuous process prepares fire retardant pre-esterification liquid, described fire retardant pre-esterification liquid is injected described second esterifier continuously, described second esterifier is horizontal esterifier, its inner chamber is divided into the first chamber from left to right, second chamber and the 3rd chamber, whipping appts is equipped with in each chamber, described fire retardant pre-esterification liquid injects described second chamber, working pressure scope in described second esterifier is 0 ~ 20kPa(G), described first, second and the 3rd operating temperature range in chamber is followed successively by 240 ~ 255 DEG C, 230 ~ 245 DEG C and 250 ~ 265 DEG C, described first, second and the 3rd reaction time in chamber is followed successively by 15 ~ 30min, 20 ~ 40min and 30 ~ 50min.
2. can directly spin the production method of copoly type Phosphorous Flame-Retardant Polyester by continuous seepage as claimed in claim 1, it is characterized in that the acid value of described fire retardant pre-esterification liquid is 95 ~ 125mgKOH/g.
3. can directly spin the production method of copoly type Phosphorous Flame-Retardant Polyester by continuous seepage as claimed in claim 1, it is characterized in that the mass content of phosphoric in described fire retardant pre-esterification liquid is not less than 3.5%.
4. can directly spin the production method of copoly type Phosphorous Flame-Retardant Polyester by continuous seepage as claimed in claim 1, it is characterized in that the mass ratio of described phosphorus flame retardant and ethylene glycol is 1:2.20 ~ 1:1.05, in the process of pre-esterification, working pressure scope is 5 ~ 20kPa(G), operating temperature range is 110 ~ 220 DEG C, and reaction time is 1 ~ 3h.
5. one kind adopt in claim 1-4 described in any one claim can continuous seepage directly spin the production method of copoly type Phosphorous Flame-Retardant Polyester can directly spin the production system of copoly type Phosphorous Flame-Retardant Polyester by continuous seepage, comprise continuous condensed Pet Production Line, described continuous condensed Pet Production Line at least comprises the first esterifier and the second esterifier that are connected successively, characterized by further comprising the pre-esterification reactor device for the preparation of fire retardant pre-esterification liquid, the outlet of described pre-esterification reactor device connects described second esterifier by pipeline, described second esterifier is horizontal esterifier, its inner chamber is divided into the first chamber from left to right, second chamber and the 3rd chamber, whipping appts is equipped with in each chamber, the outlet of described pre-esterification reactor device connects described second chamber by described pipeline.
6. can directly spin the production system of copoly type Phosphorous Flame-Retardant Polyester by continuous seepage as claimed in claim 5, it is characterized in that the pipeline between the outlet of described pre-esterification reactor device and the second esterifier being connected with fire retardant pre-esterification liquid charging tank, the pipeline between described fire retardant pre-esterification liquid charging tank and the second esterifier is provided with charging pump.
7. can directly spin the production system of copoly type Phosphorous Flame-Retardant Polyester by continuous seepage as claimed in claim 6, it is characterized in that described first chamber is connected additive material source with the 3rd chamber respectively by corresponding pipeline.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101638814A (en) * | 2008-08-01 | 2010-02-03 | 上海甲秀工业设计有限公司 | Method for manufacturing fire-retardant nine-pore polyester fibers |
| CN101671434A (en) * | 2008-09-09 | 2010-03-17 | 王忠卫 | Method for manufacturing phosphorus flame-retardant polyester |
| CN102691130A (en) * | 2012-06-19 | 2012-09-26 | 福建经纬新纤科技实业有限公司 | Process for manufacturing fire-retardant polyester fiber |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101638814A (en) * | 2008-08-01 | 2010-02-03 | 上海甲秀工业设计有限公司 | Method for manufacturing fire-retardant nine-pore polyester fibers |
| CN101671434A (en) * | 2008-09-09 | 2010-03-17 | 王忠卫 | Method for manufacturing phosphorus flame-retardant polyester |
| CN102691130A (en) * | 2012-06-19 | 2012-09-26 | 福建经纬新纤科技实业有限公司 | Process for manufacturing fire-retardant polyester fiber |
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Address after: 100037 Beijing city Haidian District Zengguang Road No. 21 Patentee after: CHINA KUNLUN CONTRACTING & ENGINEERING Corp. Patentee after: China Textile Industry Design Institute Address before: 100037 Beijing city Haidian District Zengguang Road No. 21 Patentee before: CHINA KUNLUN CONTRACTING & ENGINEERING Corp. Patentee before: China Textile Industry Design Institute |
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