CN106279266A - A kind of preparation method of liquid phosphite kind antioxidant - Google Patents
A kind of preparation method of liquid phosphite kind antioxidant Download PDFInfo
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- CN106279266A CN106279266A CN201610555884.6A CN201610555884A CN106279266A CN 106279266 A CN106279266 A CN 106279266A CN 201610555884 A CN201610555884 A CN 201610555884A CN 106279266 A CN106279266 A CN 106279266A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000007788 liquid Substances 0.000 title claims abstract description 18
- 239000003963 antioxidant agent Substances 0.000 title claims abstract description 15
- 230000003078 antioxidant effect Effects 0.000 title claims abstract description 15
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 title claims abstract description 14
- GBRSPKXOFRTAHS-UHFFFAOYSA-N 5-(4-nitrophenyl)-1,2-oxazole-3-carboxylic acid Chemical compound O1N=C(C(=O)O)C=C1C1=CC=C([N+]([O-])=O)C=C1 GBRSPKXOFRTAHS-UHFFFAOYSA-N 0.000 claims abstract description 22
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 claims abstract description 18
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 150000002148 esters Chemical group 0.000 claims abstract description 10
- 238000006467 substitution reaction Methods 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 150000001409 amidines Chemical class 0.000 claims abstract description 4
- 150000001412 amines Chemical group 0.000 claims abstract description 4
- 239000000047 product Substances 0.000 claims description 24
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 12
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical group CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 9
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 7
- 238000006555 catalytic reaction Methods 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 claims description 5
- 230000004044 response Effects 0.000 claims description 5
- SVYKKECYCPFKGB-UHFFFAOYSA-N N,N-dimethylcyclohexylamine Chemical compound CN(C)C1CCCCC1 SVYKKECYCPFKGB-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 239000006227 byproduct Substances 0.000 claims description 2
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- 239000002910 solid waste Substances 0.000 abstract 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 238000003756 stirring Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 239000012530 fluid Substances 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000284 extract Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000003039 volatile agent Substances 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010668 complexation reaction Methods 0.000 description 2
- 239000010808 liquid waste Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- XMHTUHZQDJLUSJ-UHFFFAOYSA-N Cl.OP(O)O Chemical compound Cl.OP(O)O XMHTUHZQDJLUSJ-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 150000002118 epoxides Chemical class 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- VCAFTIGPOYBOIC-UHFFFAOYSA-N phenyl dihydrogen phosphite Chemical compound OP(O)OC1=CC=CC=C1 VCAFTIGPOYBOIC-UHFFFAOYSA-N 0.000 description 1
- -1 phosphorous acyl chlorides Chemical class 0.000 description 1
- 150000004291 polyenes Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- 238000005809 transesterification reaction Methods 0.000 description 1
- 238000007039 two-step reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/141—Esters of phosphorous acids
- C07F9/145—Esters of phosphorous acids with hydroxyaryl compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention relates to the preparation method of a kind of liquid phosphite kind antioxidant, the method uses two-step method synthesis, phenol and Phosphorous chloride. are first carried out substitution reaction by the first step in the presence of a catalyst, generate intermediate triphenyl phosphite, second step uses the intermediate triphenyl phosphite generated and isooctanol to carry out ester exchange reaction, distilation obtains final products liquid diisooctyl phenyl phosphite, and wherein, described catalyst is amine or the amidine class having steric hindrance.The invention have the advantage that reaction condition is gentle, production safety coefficient is high, environmental protection, and reaction time is short, product yield is high, without solvent, not producing waste water and solid waste, course of reaction is easily controllable, raw material reusable edible, and it is high that the diisooctyl phenyl phosphite obtained has content, and acid number is low, and clear appearance is transparent, the features such as good fluidity, are particularly suitable for industrialized production.
Description
Technical field
The present invention relates to the preparation field of antioxidant, particularly to the preparation side of a kind of liquid phosphite kind antioxidant
Method.It is more particularly related to the preparation method of diisooctyl phenyl phosphite.
Background technology
Diisooctyl phenyl phosphite is a kind of liquid phosphite kind antioxidant applying excellent effect, has and is easy to pipe
Features such as mixing homogeneously with liquid form product is measured in road accumulating, convenience.In the polymer, diisooctyl phenyl phosphite can be effective
Decompose unstable per-compound, interrupt the thermo-oxidative ageing of polymer.Can at polrvinyl chloride phosphorous acid one benzene di-isooctyl
As organic auxiliary heat stabilizer, have absorption HCl concurrently, replace unstable chlorine atom and conjugated polyene sequence addition and complexation gold
Belong to ion effect, its individually in polrvinyl chloride use time without obvious stablizing effect, but with metallic soap and with after energy complexation
Metal chloride, improves thermostability and weatherability, keeps the transparency.Meanwhile, diisooctyl phenyl phosphite can also with organotin,
Epoxide and with and show good synergy, reduce main stabilizer consumption.
The preparation of the most traditional diisooctyl phenyl phosphite, is typically employed in toluene equal solvent and carries out phenol and three
The reaction of phosphorus chloride, obtains triphenyl phosphite, then normal pressure, metallic sodium catalytic action under add isooctanol carry out ester friendship
Change reaction, obtain product diisooctyl phenyl phosphite by distillation.Additionally Zhejiang chemical research institute Zheng Ying use isooctanol and
Phosphorous chloride., prepares diisooctyl phosphorous acyl chlorides with toluene as solvent, then with phenol reactant, through works such as alkali cleaning, washing, sucking filtration
Skill obtains end product.
Traditional handicraft major defect is, uses metallic sodium to make catalyst, reacts wayward, deposit in accumulating and production link
In bigger potential safety hazard；Using the organic solvents such as toluene, energy consumption cost increases, and reaction time is longer.Zhejiang chemical research institute
Technique more complicated, raw material availability is low, produce waste water the like waste more；And product is complicated, raw materials recovery difficulty
Deng.
Therefore, this area need badly and develop that a kind of safety and environmental protection, response time are short, generate without solid liquid waste, recovery former
Material reusable edible, yield are high, and the preparation method of the diisooctyl phenyl phosphite of good product quality.
Summary of the invention
The purpose of the present invention is exactly for overcoming the weak point in existing diisooctyl phenyl phosphite preparation method, and
A kind of two-step method provided prepares the technology of liquid phosphite kind antioxidant.
The purpose of the present invention can be achieved through the following technical solutions: the preparation side of a kind of diisooctyl phenyl phosphite
Method, the method uses two-step method synthesis, and the first step first carries out substitution reaction in the presence of a catalyst with phenol and Phosphorous chloride., raw
Becoming intermediate triphenyl phosphite, second step uses the intermediate generated and isooctanol to carry out ester exchange reaction, generates final producing
Product, then obtain liquid diisooctyl phenyl phosphite product through distilation.
Described process comprises the following steps that: first melted phenol and catalyst are joined four-hole boiling flask
In, drip Phosphorous chloride., control reaction temperature, time and vacuum, carry out being catalyzed substitution reaction, generate intermediate tricresyl phosphite
Phenyl ester and byproduct hydrogen chloride gas；Then adding appropriate isooctanol in four-hole boiling flask and carry out ester exchange reaction, question response is complete
The rectification unreacted isooctanol of isolated successively, the phenol of generation and target product phosphorous acid one benzene two is passed through different pungent after one-tenth
Ester, catalysis replaces and ester exchange two-step reaction all need not use solvent.
The dropping temperature of described first step catalysis substitution reaction Phosphorous chloride. is 20～45 DEG C, controls time for adding 30
～60min, vacuum degree control in the range of-0.098～0MPa, vacuum further preferably control-0.070～-
0.040MPa。
The mol ratio of described first step catalysis substitution reaction inventory is: phenol: Phosphorous chloride .=3.2～3.6:1.0.
Described catalyst can be amine or the amidine class having steric hindrance, such as triethylamine, N, N-dimethyl cyclohexyl amine, N, N-
Dimethyl benzylamine or 1,8-diazabicylo 11 carbon-7-alkene；Catalyst relative to the mass percent addition of phenol is
0.5%～1.5%.
The mol ratio of described isooctanol addition and triphenyl phosphite is 2.2～2.5:1.0, add temperature be 0～
50 DEG C, reaction temperature is 150～165 DEG C, and vacuum is-0.07～0MPa, and the response time is 5～6h.
The described isooctanol by rectification isolated and phenol are recyclable.
The rectification temperature of described diisooctyl phenyl phosphite is 185～195 DEG C, and vacuum is 0～10mmHg.
Compared with prior art, the invention have the characteristics that and replaced by catalysis and the synthesis of catalyzed transesterification two-step method
Preparation technology, uses amine under vacuum or has the amidine class of steric hindrance to make catalyst, more safety and environmental protection, and when there is reaction
Between short, course of reaction is easily controllable, without solid liquid waste generate, it is not necessary to solvent, the raw material reusable edible of recovery, raw material utilize
Rate advantages of higher, it is high that the diisooctyl phenyl phosphite obtained has content, and acid number is low, and clear appearance is transparent, good fluidity etc.
Feature.
Detailed description of the invention
Hereinafter the detailed description of the invention of the present invention is described in detail.It should be appreciated that described herein specifically
Embodiment is merely to illustrate and explains the present invention, is not limited to the present invention.
Embodiment 1
In the 250ml four-hole boiling flask equipped with stirring, thermometer, condensing unit and HCl gas absorbing device, add
72.79g phenol, 0.7g catalyst 1,8-diazabicylo 11 carbon-7-alkene, open stirring, control temperature is at 20 DEG C, under normal pressure
Dropping 29.51g Phosphorous chloride., controls rate of addition, within about 30 minutes, drips off, completion of dropwise addition, keeps reaction 2h, afterwards at 35 DEG C
It is to slowly warm up to 150 DEG C, controls vacuum-0.050MPa, constantly extract the HCl gas generated out, and use alkali liquor absorption.The first step
It is cooled to 40 DEG C after having reacted, adds 78.12g isooctanol, and add 0.5g catalyst 1,8-diazabicylo 11 carbon-7-
Alkene, is warming up to 155 ± 5 DEG C and keeps reaction 2h, then start progressively to be evacuated to-0.07MPa, react 5h under normal pressure.React
Start after one-tenth distillation, front-end volatiles not Wei isooctanol and phenol, be 185～195 DEG C in temperature, vacuum is 0～10mmHg condition
Lower target product diisooctyl phenyl phosphite is stably steamed, the available as clear as crystal fluid product of 77.50g, produce after measured
Product acid number is 0.03mgKOH/g, and relative density (25 DEG C) is 0.947, and index of refraction (20 DEG C) is 1.475.
Embodiment 2
In the 250ml four-hole boiling flask equipped with stirring, thermometer, condensing unit and HCl gas absorbing device, add
72.79g phenol, 0.5g catalyst of triethylamine, open stirring, control temperature, at 30 DEG C, drips 29.51g Phosphorous chloride. under normal pressure,
Control rate of addition, within about 45 minutes, drip off, completion of dropwise addition, at 30 DEG C, keep reaction 2h, be to slowly warm up to 150 DEG C afterwards, control
Vacuum-0.070MPa processed, constantly extracts the HCl gas generated out, and uses alkali liquor absorption.The first step is cooled to 40 after having reacted
DEG C, add 78.12g isooctanol, and add be warming up under 0.5g catalyst of triethylamine, normal pressure 155 ± 5 DEG C keep reaction 2h, so
Rear beginning is progressively evacuated to-0.07MPa, reacts 5h.Start after having reacted distillation, front-end volatiles not Wei isooctanol and phenol,
Being 185～195 DEG C in temperature, vacuum is stably to be steamed by target product diisooctyl phenyl phosphite under the conditions of 0～10mmHg
Going out, the available as clear as crystal fluid product of 78.02g, product acid number is 0.05mgKOH/g after measured, and relative density (25 DEG C) is
0.946, index of refraction (20 DEG C) is 1.478.
Embodiment 3
In the 250ml four-hole boiling flask equipped with stirring, thermometer, condensing unit and HCl gas absorbing device, add
72.79g phenol, 0.7g catalyst n, N-dimethyl cyclohexyl amine, open stirring, control temperature, at 45 DEG C, drips under normal pressure
29.51g Phosphorous chloride., controls rate of addition, within about 45 minutes, drips off, completion of dropwise addition, keeps reaction 1h, the most slowly at 40 DEG C
It is warming up to 150 DEG C, controls vacuum-0.040MPa, constantly extract the HCl gas generated out, and use alkali liquor absorption.The first step is reacted
It is cooled to 50 DEG C after completing, adds 78.12g isooctanol, and add 0.5g catalyst n, N-dimethyl cyclohexyl amine, heats up under normal pressure
Keep reaction 2h to 160 ± 5 DEG C, then start progressively to be evacuated to-0.07MPa, react 5h.Distillation is started after having reacted,
Front-end volatiles not Wei isooctanol and phenol, be 185～195 DEG C in temperature, vacuum is target product is sub-under the conditions of 0～10mmHg
Phosphoric acid one benzene di-isooctyl stably steams, and the available as clear as crystal fluid product of 77.32g, product acid number is after measured
0.03mgKOH/g, relative density (25 DEG C) is 0.950, and index of refraction (20 DEG C) is 1.478.
Comparative example 1
Such as the preparation method of the diisooctyl phenyl phosphite in embodiment 1, except that, the first step does not use and urges
Agent, finally steams the target product as clear as crystal fluid product of diisooctyl phenyl phosphite 52.60g, product acid number after measured
For 1.32mgKOH/g, relative density (25 DEG C) is 0.958, and index of refraction (20 DEG C) is 1.484.
Comparative example 2
Such as the preparation method of the diisooctyl phenyl phosphite in embodiment 1, except that, second step ester exchange is often
Pressure is carried out (0.1MPa), finally steams the target product as clear as crystal fluid product of diisooctyl phenyl phosphite 40.27g, warp
Measuring product acid number is 0.09mgKOH/g, and relative density (25 DEG C) is 0.957, and index of refraction (20 DEG C) is 1.486.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited in above-mentioned embodiment
Detail, in the technology concept of the present invention, technical scheme can be carried out multiple simple variant, this
A little simple variant belong to protection scope of the present invention.
It is further to note that each the concrete technical characteristic described in above-mentioned detailed description of the invention, at not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to various can
The compound mode of energy illustrates the most separately.
Additionally, combination in any can also be carried out between the various different embodiment of the present invention, as long as it is without prejudice to this
The thought of invention, it should be considered as content disclosed in this invention equally.
Claims (8)
1. the preparation method of a liquid phosphite kind antioxidant, it is characterised in that: the method uses two-step method to synthesize, and first
Phenol and Phosphorous chloride. are first carried out substitution reaction by step in the presence of a catalyst, generate intermediate triphenyl phosphite, second step
Using the intermediate triphenyl phosphite generated and isooctanol to carry out ester exchange reaction, it is sub-that distilation obtains final products liquid
Phosphoric acid one benzene di-isooctyl, wherein, described catalyst is amine or the amidine class having steric hindrance.
The preparation method of liquid phosphite kind antioxidant the most according to claim 1, it is characterised in that the tool of the method
Body technology comprises the following steps: join in four-hole boiling flask by melted phenol and catalyst, drips Phosphorous chloride., controls reaction
Temperature, time and vacuum, carry out being catalyzed substitution reaction, generate intermediate triphenyl phosphite and byproduct hydrogen chloride gas；
Then adding appropriate isooctanol in four-hole boiling flask and carry out ester exchange reaction, question response passes through rectification isolated successively after completing
Unreacted isooctanol, the phenol of generation and target product diisooctyl phenyl phosphite, catalysis replaces and ester exchange two step is anti-
Should all need not use solvent.
The preparation method of liquid phosphite kind antioxidant the most according to claim 1 and 2, it is characterised in that described
The dropping temperature of catalysis substitution reaction Phosphorous chloride. is 20～45 DEG C, and time for adding controls 30～60min, vacuum degree control
In the range of-0.098～0MPa.
The preparation method of liquid phosphite kind antioxidant the most according to claim 1 and 2, it is characterised in that described
The mol ratio of catalysis substitution reaction inventory is: phenol: Phosphorous chloride .=3.2～3.6:1.0.
The preparation method of liquid phosphite kind antioxidant the most according to claim 1 and 2, it is characterised in that described
Catalyst is triethylamine, N, N-dimethyl cyclohexyl amine, N, in N-dimethyl benzylamine and 1,8-diazabicylo 11 carbon-7-alkene
One or more；Described catalyst is 0.5%～1.5% relative to the addition of phenol.
The preparation method of liquid phosphite kind antioxidant the most according to claim 1 and 2, it is characterised in that described
Isooctanol addition is 2.2～2.5:1.0 with the mol ratio of triphenyl phosphite, and adding temperature is 0～50 DEG C, and reaction temperature is
150～165 DEG C, vacuum is-0.07～0MPa, and the response time is 5～6h.
The preparation method of liquid phosphite kind antioxidant the most according to claim 2, it is characterised in that described passes through
The isooctanol of rectification isolated, phenol are recyclable.
The preparation method of liquid phosphite kind antioxidant the most according to claim 1 and 2, it is characterised in that described
The rectification condition of diisooctyl phenyl phosphite includes: temperature is 185～195 DEG C, and vacuum is 0～10mmHg.
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Cited By (5)
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| CN106977542A (en) * | 2017-05-26 | 2017-07-25 | 南通艾德旺化工有限公司 | A kind of preparation method of triphenyl phosphite |
| CN109354772A (en) * | 2018-10-26 | 2019-02-19 | 安庆市悦发管业有限公司 | A kind of preparation method of uvioresistant PE coil pipe material |
| CN110885474A (en) * | 2019-12-12 | 2020-03-17 | 梁山新翔新材料有限公司 | Preparation method and application of phosphite antioxidant |
| CN111607963A (en) * | 2020-05-27 | 2020-09-01 | 浙江恒澜科技有限公司 | Polyester filament POY oiling agent and preparation method thereof |
| CN114075240A (en) * | 2020-08-18 | 2022-02-22 | 张家港市国泰华荣化工新材料有限公司 | Synthesis method of tris (1, 1,1,3,3, 3-hexafluoro-2-propyl) phosphorous acid |
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| CN110885474A (en) * | 2019-12-12 | 2020-03-17 | 梁山新翔新材料有限公司 | Preparation method and application of phosphite antioxidant |
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| CN114075240A (en) * | 2020-08-18 | 2022-02-22 | 张家港市国泰华荣化工新材料有限公司 | Synthesis method of tris (1, 1,1,3,3, 3-hexafluoro-2-propyl) phosphorous acid |
| CN114075240B (en) * | 2020-08-18 | 2023-11-17 | 张家港市国泰华荣化工新材料有限公司 | Synthesis method of tri (1, 3-hexafluoro-2-propyl) phosphorous acid |
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