CN106316941A - Method for continuous neutralization and water separation of polycondensation liquid in production process of antioxidant TMQ - Google Patents
Method for continuous neutralization and water separation of polycondensation liquid in production process of antioxidant TMQ Download PDFInfo
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- 239000007788 liquid Substances 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000006068 polycondensation reaction Methods 0.000 title claims abstract description 44
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 238000006386 neutralization reaction Methods 0.000 title abstract description 10
- 239000003963 antioxidant agent Substances 0.000 title abstract description 9
- 230000003078 antioxidant effect Effects 0.000 title abstract description 8
- 238000000926 separation method Methods 0.000 title abstract 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000011259 mixed solution Substances 0.000 claims abstract description 23
- 230000003068 static effect Effects 0.000 claims abstract description 15
- 239000002351 wastewater Substances 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 63
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 21
- 239000012043 crude product Substances 0.000 claims description 17
- 238000000605 extraction Methods 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 230000003139 buffering effect Effects 0.000 claims description 6
- 239000012071 phase Substances 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- 239000001488 sodium phosphate Substances 0.000 claims description 4
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 4
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 4
- 239000008346 aqueous phase Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000011736 potassium bicarbonate Substances 0.000 claims description 2
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 2
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 235000011181 potassium carbonates Nutrition 0.000 claims description 2
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 2
- 235000011118 potassium hydroxide Nutrition 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 235000011008 sodium phosphates Nutrition 0.000 claims description 2
- 230000000087 stabilizing effect Effects 0.000 claims description 2
- NOYPYLRCIDNJJB-UHFFFAOYSA-N trimetrexate Chemical compound COC1=C(OC)C(OC)=CC(NCC=2C(=C3C(N)=NC(N)=NC3=CC=2)C)=C1 NOYPYLRCIDNJJB-UHFFFAOYSA-N 0.000 claims 11
- 238000007599 discharging Methods 0.000 abstract description 6
- 239000003513 alkali Substances 0.000 abstract description 2
- 230000008901 benefit Effects 0.000 abstract description 2
- 238000009833 condensation Methods 0.000 abstract description 2
- 230000005494 condensation Effects 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 230000003472 neutralizing effect Effects 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 abstract description 2
- 230000002378 acidificating effect Effects 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 239000000178 monomer Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000004821 distillation Methods 0.000 description 4
- 230000008676 import Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000003377 acid catalyst Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- SHOJXDKTYKFBRD-UHFFFAOYSA-N 4-Methyl-3-penten-2-one, 9CI Chemical compound CC(C)=CC(C)=O SHOJXDKTYKFBRD-UHFFFAOYSA-N 0.000 description 1
- 238000007171 acid catalysis Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- -1 ketone amines Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D215/00—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems
- C07D215/02—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen atoms or carbon atoms directly attached to the ring nitrogen atom
- C07D215/04—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen atoms or carbon atoms directly attached to the ring nitrogen atom with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to the ring carbon atoms
- C07D215/06—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen atoms or carbon atoms directly attached to the ring nitrogen atom with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to the ring carbon atoms having only hydrogen atoms, hydrocarbon or substituted hydrocarbon radicals, attached to the ring nitrogen atom
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A method for continuous neutralization and water separation of a TMQ polycondensation liquid in the production process of an antioxidant TMQ comprises the following steps: 1, carrying out buffer storage on the TMQ polycondensation liquid obtained after condensation and polymerization of aniline and acetone (or derivatives thereof) under an acidic condition in the production process of the two-step method or one-step method antioxidant TMQ; 2, mixing the TMQ polycondensation liquid with a liquid alkali; 3, discharging the above obtained mixed solution from a static mixer, and continuously neutralizing the mixed solution in a two-stage neutralization kettle; and 4, layering the TMQ neutralized solution in a water separator, extracting crude antioxidant TMQ from the obtained upper layer, and extracting TMQ wastewater from the obtained lower layer. The method has the advantages of complete realization of continuous operation and DCS control of neutralization and water separation of the TMQ polycondensation liquid in the production process of the antioxidant TMQ, great reduction of the labor intensity, saving of manpower cost, and improvement of the stability of the production process of the antioxidant TMQ.
Description
Technical field
The invention belongs to technical field of fine, relate in a kind of age resistor TMQ production processTMQThe processing method that polycondensation liquid neutralizes continuously, is the preparation technology of a kind of environmental protection.
Background technology
Age resistor TMQ is 2,2,4-trimethyls-1; the two of 2-dihyaroquinoline, three, four polymers, have another name called anti-aging agent RD, be a kind of ketone amines antioxidants; it is mainly used as rubber antioxidant for faint yellow to ruins pool coloured particles or thin slice, is one of rubber antioxidant product of having the call on domestic and international market.
The synthesis of age resistor TMQ is by aniline and acetone (or derivatives thereof), under acid catalyst effect, 2 are generated by condensation reaction, 2,4-trimethyl-1,2-dihyaroquinoline monomer, then the monomer of gained polyreaction under acid catalyst effect becomes dimer or three, four polymers and polymer etc., alkali neutralizes, point water, and oil phase carries out distillation and obtains age resistor TMQ.
The synthesis of age resistor TMQ can be divided into " one-step method " and " two-step method "." two-step method " is that first condensation prepares 2,2,4-trimethyl-1,2-dihyaroquinoline monomer, after removing reaction water, unreacted reactant and other low-boiling-point substance, then carries out the polymerization of monomer in acid condition, neutralizes, oil phase distillation obtains TMQ finished product；And " one-step method " is to make 2,2,4-trimethyls-1, the preparation of 2-dihyaroquinoline monomer and the same reactor of polyreaction complete to obtain the polycondensation liquid of TMQ simultaneously, then in polycondensation liquid liquid caustic soda and after, then separate unnecessary reactant and other low-boiling-point substance, obtain TMQ finished product.Two-step process process is long, consumes big, but the working substance content in products obtained therefrom is high；And one-step method process is simple, consumes little, but working substance content is low.
Simultaneously in order to make reaction carry out to the direction of beneficially product, it is necessary to being removed from response system in time by water generation reaction, condensation reaction the most all uses the solvent azeotropic band water that boiling point is higher.If so dividing whether adding water entrainer, the big class of " having solvent method " and " solventless method " two can be divided into again.Use toluene equal solvent reaction water to be taken out of, beneficially the neutralization of subsequent reactions liquid, point water, but add the cost such as equipment and operation.
In the industrial preparative method of traditional age resistor TMQ, either one-step method or two-step method, all use the still reaction method of interval, that is: raw material and catalyst (and solvent etc.) being thrown into quantitatively in reactor, reaction obtains TMQ polycondensation liquid after terminating, then proceeds to TMQ polycondensation liquid neutralize and drip in quantitative liquid caustic soda and acid catalyst in still, after reaching the pH value of requirement, point water after stratification, the aqueous phase separated is TMQ waste water, carries out reclaiming post processing；Oil phase is TMQ crude product (is mainly composed of 2,2,4-trimethyl-1, the monomer of 2-dihyaroquinoline and two, three, four polymers, aniline, acetone, isopropylidene acetone etc.), goes distillation system distillation to obtain age resistor TMQ.
Due in time of polycondensation reaction and polycondensation liquid and the difference of required time, a usual neutralization still need to process the material (TMQ polycondensation liquid) of 2-4 reactor, by multiple reactors and the handover operation of neutralization still, although having reached semi-continuous operating procedure, but this technique there is also defect:
(1) process is semicontinuous, even if technical process enters DCS system, need remain for manually to reactor, neutralize and carry out ceaselessly handover operation between still, wherein step includes: neutralize the charging of still polycondensation liquid, the preparation of liquid caustic soda and dropping, stirring neutralizes, neutralize after standing and point water (including TMQ crude product discharging and TMQ waste water discharging) etc..
(2) during, the control of pH value is to use manual site to hang sample analysis, brings to production management certain loaded down with trivial details, too increases human cost.
(3) need repeatedly to add liquid caustic soda, repeatedly sampling and measuring pH value during the adjustment of pH value.
Above 3 complex operations, constrain the seriality of process, add the labour costs of production, have impact on the stability of product simultaneously.
Summary of the invention
Defect that the purpose of the present invention is contemplated to overcome above-mentioned prior art to exist and a kind of stability that improves is provided, improve neutralize, in the age resistor TMQ production process of point water efficiency and effect TMQ polycondensation liquid neutralize, the continuous treatment method of point water.
The purpose of the present invention can be achieved through the following technical solutions:
In age resistor TMQ production process, polycondensation liquid neutralizes and the continuous treatment method of point water, it is characterised in that the method comprises the following steps:
(1), in the production process of the age resistor TMQ such as " two-step method " or " one-step method ", aniline and acetone (or derivatives thereof) carry out being condensed and being polymerized the polycondensation liquid obtaining TMQ in acid condition, are placed in vat by the polycondensation liquid of this TMQ, and buffering is deposited；
(2) with liquid caustic soda, above-mentioned TMQ polycondensation liquid is imported static mixer to mix, obtain mixed solution；
(3) mixed solution neutralizes with still from static mixer the most afterwards in two-stage continuously, exports be provided with online pH meter with still in two-stage, and it is 7-11 that on-line control controls the pH value of solution, i.e. obtains the TMQ neutralizer that pH value is qualified；
(4), during TMQ neutralizer continuous print enters water knockout drum, it is layered in water knockout drum, water knockout drum upper strata continuous print extraction oil phase, is age resistor TMQ crude product；Water knockout drum lower floor continuous print extraction aqueous phase, is TMQ waste water.
The described TMQ polycondensation liquid in step (2) and the addition of liquid caustic soda are controlled by effusion meter and regulation valve.
The described liquid caustic soda in step (2) includes sodium hydroxide, sodium carbonate, sodium bicarbonate, potassium hydroxide, potassium carbonate, potassium bicarbonate, sodium phosphate, dibastic sodium phosphate and solution thereof or mixed solution.
By potential difference, from the first order and still flows in the second level and still the described mixed solution in step (3).
The described two-stage in step (3) includes stirring, heating and stabilizing control system etc. with still.
The described TMQ neutralizer in step (4) is flowed in water knockout drum with still from the second level by potential difference.
The signal of described effusion meter, regulation valve and pH meter is automatically controlled by dcs.
The present invention is in age resistor TMQ production processTMQPolycondensation liquid neutralizes continuously, the processing method of point water, the mode utilizing static mixer and reactor to combine realizes TMQ and neutralizes continuously, divides water continuously, serialization obtain TMQ crude product and TMQ waste water, substitute the operation of intermittent still reaction, realize TMQ and produce the automatization neutralizing, dividing water process, labor intensity can be reduced and reduce production cost, keep producing and the stability of product quality.
Compared with prior art, invention fully achieves continuous operation and DCS controls, it is achieved that the mensuration of on-line continuous pH value, go to control TMQ polycondensation liquid, the proportioning of liquid caustic soda with the pH value signal measured simultaneously, have the advantage that
(1) present invention is continuous process, compared with batch technology, solves the neutralization of TMQ polycondensation liquid and the serialization problem of point water always perplexing plant produced, labor intensity can be greatly reduced, saved human cost；
(2) improve the stability of age resistor TMQ production process；
(3) achieving DCS to automatically control, charging have employed burden control；
(4) have employed static mixer, substantially improve mixed effect, beneficially the stability of pH value；
(5) achieve the mensuration of on-line pH value, and go to control charging proportioning with this signal.
Accompanying drawing explanation
Fig. 1 is the general flow chart that the TMQ polycondensation liquid of the embodiment of the present invention neutralized, divided continuously water continuously.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the method for the present invention is described in further detail.
Following example see accompanying drawing 1, in continuous tower-type reacts, specifically, it is simply that utilize fixed bed or trickle bed, tower reactor etc., and load filler in the reactor.Being seated in reaction tower by aniline, aniline, acetone and hydrochloric acid carry out successive reaction from tower bottom or bottom continuous feed, aniline and acetone in being in fixed bed under hydrochloric acid catalysis effect.
Embodiment
1
(1) by the production process of the age resistor TMQ such as " two-step method " or " one-step method ", aniline and acetone carry out being condensed and being polymerized the polycondensation liquid obtaining TMQ in acid condition, are placed in vat, and buffering is deposited.
(2) utilize dcs (DCS system) according to pH=7, control to import static mixer after TMQ polycondensation liquid is tentatively carried out proportioning with liquid caustic soda with regulation valve by effusion meter and mix, obtain mixed solution.
(3) mixed solution neutralizes with still from static mixer the most afterwards in the first order continuously, owing to the reason of polycondensation step causes concentration of hydrochloric acid in polycondensation liquid too high, pH meter is measured in outflow one-level and the pH value of still material is on the low side, by potential difference, from the first order and still flows in the second level and still mixed solution, DCS strengthens the flow of liquid caustic soda automatically by the proportioning Adjusted Option set, proceed to neutralize, obtain the qualified TMQ neutralizer of pH=7.
(4) during TMQ neutralizer continuous print enters water knockout drum, water knockout drum upper strata continuous print extraction age resistor TMQ crude product；Water knockout drum lower floor continuous print extraction TMQ waste water.Age resistor TMQ crude product pH=7, wherein water content 2.34% after testing；TMQ wastewater pH=7, wherein age resistor TMQ content in crude product 1.02%.
Embodiment
2
(1) by the production process of the age resistor TMQ such as " two-step method " or " one-step method ", aniline and acetone carry out being condensed and being polymerized the polycondensation liquid obtaining TMQ in acid condition, are placed in vat, and buffering is deposited.
(2) utilize dcs (DCS system) according to pH=9, control to import static mixer after TMQ polycondensation liquid is tentatively carried out proportioning with liquid caustic soda with regulation valve by effusion meter and mix, obtain mixed solution.
(3) mixed solution neutralizes with still from static mixer the most afterwards in the first order continuously, owing to the reason of TMQ polycondensation step causes concentration of hydrochloric acid in polycondensation liquid too low, pH meter is measured in outflow one-level and the pH value of still material is higher, by potential difference, from the first order and still flows in the second level and still mixed solution, DCS reduces the flow of liquid caustic soda automatically by the proportioning Adjusted Option set, proceed to neutralize, obtain the qualified TMQ neutralizer of pH=9.
(4) during TMQ neutralizer continuous print enters water knockout drum, water knockout drum upper strata continuous print extraction age resistor TMQ crude product；Water knockout drum lower floor continuous print extraction TMQ waste water, age resistor TMQ crude product pH=9, wherein water content 2.24% after testing；TMQ wastewater pH=9, wherein age resistor TMQ content in crude product 2.15%.
Embodiment
3
(1) by the production process of the age resistor TMQ such as " two-step method " or " one-step method ", aniline and acetone carry out being condensed and being polymerized the polycondensation liquid obtaining TMQ in acid condition, are placed in vat, and buffering is deposited.
(2) utilize dcs (DCS system) according to pH=11, control to import static mixer after TMQ polycondensation liquid is tentatively carried out proportioning with liquid caustic soda with regulation valve by effusion meter and mix, obtain mixed solution.
(3) mixed solution neutralizes with still from static mixer the most afterwards in the first order continuously, pH meter is measured in outflow one-level and the pH value of still material is too high, by potential difference, from the first order and still flows in the second level and still mixed solution, it is the most higher that the pH meter in Zhong Hefu exit, the second level records discharging pH value, DCS adds TMQ polycondensation liquid automatically by the proportioning set, the additional amount of TMQ polycondensation liquid is controlled by constantly measuring the pH value of two grades of neutralization still dischargings, make the pH=11 of mixed solution discharging in two grades of neutralization stills, the qualified TMQ neutralizer obtained.
(4) during TMQ neutralizer continuous print enters water knockout drum, water knockout drum upper strata continuous print extraction age resistor TMQ crude product；Water knockout drum lower floor continuous print extraction TMQ waste water, age resistor TMQ crude product pH=11, wherein water content 2.75% after testing；TMQ wastewater pH=11, wherein age resistor TMQ content in crude product 2.11%.
Embodiment
4
(1) by the production process of the age resistor TMQ such as " two-step method " or " one-step method ", aniline and acetone carry out being condensed and being polymerized the polycondensation liquid obtaining TMQ in acid condition, are placed in vat, and buffering is deposited.
(2) utilize dcs (DCS system) according to pH=10, control to import static mixer after TMQ polycondensation liquid is tentatively carried out proportioning with liquid caustic soda with regulation valve by effusion meter and mix, obtain mixed solution.
(3) mixed solution neutralizes with still from static mixer the most afterwards in the first order continuously, owing to the content of this batch of raw material liquid caustic soda is higher, cause pH meter to measure in outflow one-level and the pH value of still material is higher, by potential difference, from the first order and still flows in the second level and still mixing mixed solution, DCS reduces the flow of liquid caustic soda automatically by the proportioning Adjusted Option set, proceed to neutralize, obtain the qualified TMQ neutralizer of pH=10.
(4) during TMQ neutralizer continuous print enters water knockout drum, water knockout drum upper strata continuous print extraction age resistor TMQ crude product；Water knockout drum lower floor continuous print extraction TMQ waste water, age resistor TMQ crude product pH=10, wherein water content 1.45% after testing；TMQ wastewater pH=10, wherein age resistor TMQ content in crude product 0.92%.
Although the present invention is illustrated with embodiment referring to the drawings, it will be clear that for a person skilled in the art, on the premise of without departing substantially from the spirit and scope of the present invention, the present invention can be made various modifications and variations.Therefore, the various changes of the present invention, change are contained by the content of appending claims and equivalent thereof.
Claims (7)
1. the method that in age resistor TMQ production process, polycondensation liquid neutralizes continuously, divides water continuously, it is characterized in that, the method comprises the following steps: in the production process of (1) " two-step method " or " one-step method " age resistor TMQ, aniline and acetone (or derivatives thereof) carry out being condensed and be polymerized the polycondensation liquid obtaining TMQ in acid condition, being placed in vat by the polycondensation liquid of this TMQ, buffering is deposited；(2) with liquid caustic soda, above-mentioned TMQ polycondensation liquid is imported static mixer to mix, obtain mixed solution；(3) mixed solution neutralizes with still from static mixer the most afterwards in two-stage continuously, exports be provided with online pH meter with still in two-stage, and it is 7-11 that on-line control controls the pH value of solution, i.e. obtains the TMQ neutralizer that pH value is qualified；(4), during TMQ neutralizer continuous print enters water knockout drum, it is layered in water knockout drum, water knockout drum upper strata continuous print extraction oil phase, is age resistor TMQ crude product；Water knockout drum lower floor continuous print extraction aqueous phase, is TMQ waste water.
Method the most according to claim 1, is characterized in that the addition of the TMQ polycondensation liquid in described step (2) and liquid caustic soda is controlled by effusion meter and regulation valve.
Method the most according to claim 1, is characterized in that the liquid caustic soda in described step (2) is sodium hydroxide, sodium carbonate, sodium bicarbonate, potassium hydroxide, potassium carbonate, potassium bicarbonate, sodium phosphate, dibastic sodium phosphate one or more mixed solution therein.
Method the most according to claim 1, is characterized in that from the first order and still flows in the second level and still the mixed solution in described step (3) by potential difference.
Method the most according to claim 1, is characterized in that in the two-stage in described step (3) and still includes stirring, heating and stabilizing control system.
Method the most according to claim 1, is characterized in that the TMQ neutralizer in described step (4) is flowed in water knockout drum with still from the second level by potential difference.
7., according to the method one of claim 1-6 Suo Shu, it is characterized in that the signal of described effusion meter, regulation valve and pH meter is automatically controlled by dcs.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108610230A (en) * | 2018-03-09 | 2018-10-02 | 惠州大亚湾伊科思新材料科技发展有限公司 | A kind of method and apparatus controlling styrene pH value after styrene extraction device decolourizes |
| CN109665991A (en) * | 2017-10-16 | 2019-04-23 | 中国石油化工股份有限公司 | A kind of preparation method of anti-aging agent TMQ |
| CN110590657A (en) * | 2019-09-16 | 2019-12-20 | 山东尚舜化工有限公司 | Equipment and process for full-automatic continuous production of antioxidant RD |
| CN113735766A (en) * | 2020-05-27 | 2021-12-03 | 中石化南京化工研究院有限公司 | Preparation method of anti-aging agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109665991A (en) * | 2017-10-16 | 2019-04-23 | 中国石油化工股份有限公司 | A kind of preparation method of anti-aging agent TMQ |
| CN109665991B (en) * | 2017-10-16 | 2022-08-23 | 中国石油化工股份有限公司 | Preparation method of anti-aging agent TMQ |
| CN108610230A (en) * | 2018-03-09 | 2018-10-02 | 惠州大亚湾伊科思新材料科技发展有限公司 | A kind of method and apparatus controlling styrene pH value after styrene extraction device decolourizes |
| CN110590657A (en) * | 2019-09-16 | 2019-12-20 | 山东尚舜化工有限公司 | Equipment and process for full-automatic continuous production of antioxidant RD |
| CN110590657B (en) * | 2019-09-16 | 2020-11-17 | 山东尚舜化工有限公司 | Equipment and process for full-automatic continuous production of antioxidant RD |
| CN113735766A (en) * | 2020-05-27 | 2021-12-03 | 中石化南京化工研究院有限公司 | Preparation method of anti-aging agent |
| CN113735766B (en) * | 2020-05-27 | 2023-08-29 | 中国石油化工股份有限公司 | Preparation method of anti-aging agent |
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