CN1162402C - Process for equipment for continuously preparing diazonium salt of triarylamine - Google Patents
Process for equipment for continuously preparing diazonium salt of triarylamine Download PDFInfo
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- CN1162402C CN1162402C CNB011052554A CN01105255A CN1162402C CN 1162402 C CN1162402 C CN 1162402C CN B011052554 A CNB011052554 A CN B011052554A CN 01105255 A CN01105255 A CN 01105255A CN 1162402 C CN1162402 C CN 1162402C
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- triarylamine
- diazonium salt
- sodium nitrite
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Abstract
The present invention discloses a method for continuously preparing diazonium salt of triarylamine and a device for realizing the method. The present invention has the technical scheme that a mixed solution of triarylamine and acid and a sodium nitrite solution are continuously input to the bottom of a tubular reactor with a cooling jacket; reaction products flow out of the top of the tubular reactor; the proportion of reaction material of each section of the tubular reactor is constant by seriously controlling the charge proportion of the triarylamine, sulfuric acid or hydrochloric acid, and the sodium nitrite; thus, the present invention has the advantages that the defect of diazonium salt decomposition resulting from non-uniform local concentration and high temperature in the prior art is overcome, and the production efficiency is enhanced.
Description
The present invention relates to the preparation method of diazonium salt of triarylamine.
Diazonium salt of triarylamine is a kind of important intermediate, is the main raw material of synthesizing guaiacol as the diazonium salt of Ortho Anisidine.
Present industrial preparation diazonium salt of triarylamine be in reactor, carry out the batch production method, as Chinese patent 95120316 and 95101653 disclosed technology.There are many defectives that are difficult to overcome in this batch production method:
The preparation of diazonium salt of triarylamine is general to be raw material with uncle's arylamine all, and uncle's arylamine is dissolved in the strong acid, adds sodium nitrite solution then, Sodium Nitrite and strong acid reaction, generate nitrous acid, nitrous acid carries out diazotization reaction with uncle's arylamine then, generates diazonium salt of triarylamine.In above-mentioned reaction process, should strict amount and the control reaction temperature of controlling nitrous acid.The consumption of acid is excessive a little, but can not too excessive, otherwise the diazonium salt of triarylamine of generation will be decomposed again; Because diazonium salt at high temperature decomposes easily, and the preparation of diazonium salt is a thermopositive reaction, so production process is quite high to the requirement of conducting heat.For general stirred autoclave, no matter adopt what method to stir, all exist local acid concentration too high and cross low and reactor in the uneven temperature phenomenon, the diazonium salt that causes generation decomposes again and reduces formation efficiency.
Therefore, provide a kind of new method for preparing diazonium salt of triarylamine, will have crucial meaning.
One of purpose of the present invention is to disclose a kind of method of continuously preparing diazonium salt of triarylamine, to overcome the above-mentioned defective of prior art;
Two of purpose of the present invention is the device of open realization aforesaid method.
Realize the technical scheme of the object of the invention:
The said method of the present invention comprises the steps:
Uncle's arylamine is imported a bottom that has first tubular reactor of cooling jacket with the mixing solutions of sulfuric acid or hydrochloric acid continuously with sodium nitrite solution, in this reactor, Sodium Nitrite at first reacts with sulfuric acid or hydrochloric acid, generate nitrous acid, nitrous acid carries out diazotization reaction with uncle's arylamine then, generate diazonium salt of triarylamine, the final reaction product is from the top outflow reactor of tubular reactor.
Temperature of reaction is generally 0～50 ℃;
The charge proportion of first tubular reactor is:
Uncle's arylamine: sulfuric acid or hydrochloric acid: Sodium Nitrite=1: (1～8): (1～1.1);
The residence time of material in reactor is 0.5～60s.
For enhancing productivity, can make the reaction product that flows out the first tubular reactor top cool off, and replenish the bottom that enters second reactor that has cooling jacket behind the sodium nitrite solution again by a water cooler, so that do not have uncle's arylamine continuation of having reacted and the nitrous acid that replenishes to react, to improve reaction efficiency.At last, synthetic diazonium salt of triarylamine solution flows out from the top of second reactor, and partial reflux enters first tubular reactor again with mixing solutions, the sodium nitrite solution of arylamine, sulfuric acid or hydrochloric acid, and part enters follow-up workshop section as finished product.
By above-mentioned disclosed technical scheme as seen:
Above-mentioned reaction process is carried out in flow process, reaction solution obtains thorough mixing, as long as the charge proportion of strict control uncle arylamine, sulfuric acid or hydrochloric acid, Sodium Nitrite, carrying out along with reaction, the ratio of the reaction mass in each cross section of tubular reactor all is constant, thereby has overcome the uneven defective of existing in prior technology partial concn;
Adopt the tubular reactor with cooling jacket simultaneously, can improve heat transfer efficiency, control reaction temperature effectively is to avoid causing owing to temperature is too high the decomposition of diazonium salt.
The device of realizing aforesaid method comprises:
First tubular reactor that has cooling jacket;
Second tubular reactor that has cooling jacket, the outlet of this reactor is connected with the inlet of the follow-up workshop section and first tubular reactor;
A water cooler that is connected with the first tubular reactor top exit and the second tubular reactor bottom inlet respectively;
A feedstock pump and a nitrous acid sodium pump all are connected by the bottom inlet of pipeline with first reactor; Said feedstock pump is used for the mixing solutions of uncle's arylamine and sulfuric acid or hydrochloric acid is sent into first reactor, and said nitrous acid sodium pump is used for sodium nitrite solution is gone into first reactor; The nitrous acid sodium pump also is connected by the inlet of pipeline with second reactor bottom simultaneously, to replenish Sodium Nitrite.
Below by accompanying drawing the present invention is narrated.
Fig. 1 is the schema of continuously preparing diazonium salt of triarylamine.
Fig. 2 is the structure of reactor synoptic diagram.
As seen from Figure 1, the said method of the present invention comprises the steps:
The mixed solution of uncle's arylamine and sulfuric acid or hydrochloric acid passes through nitrous by feedstock pump 1, sodium nitrite solution Acid sodium pump 2 is imported one together continuously with the bottom of first tubular reactor 3 of cooling jacket, In this reactor 3, natrium nitrosum at first reacts with sulfuric acid or hydrochloric acid, generates nitrous acid, and is then inferior Nitric acid carries out diazo-reaction with uncle's arylamine, generates diazonium salt of triarylamine, and the final reaction product is anti-from tubular type Answer the top of device 3 to flow out.
The product that flows out first tubular reactor, 3 tops is cooled off, also by a cooler 4 Enter again the bottom with second reactor 5 of cooling jacket behind the additional sodium nitrite solution, so that do not have The uncle's arylamine that has reacted continues to react with the nitrous acid that replenishes, to improve reaction efficiency. At last, close The diazonium salt of triarylamine solution that becomes flows out from the top of second reactor 5, and partial reflux is with arylamine, sulphur The mixed solution of acid or hydrochloric acid, sodium nitrite solution enter first tubular reactor 3 together again, and part is done For finished product enters follow-up workshop section.
Above-mentioned first tubular reactor 3 and second tubular reactor 5 with cooling jacket can preferably be adopted With structure as shown in Figure 2.
As seen from Figure 2, said reactor comprises:
A cylindrical shell 6;
An inner casing 7 concentric with housing 6 forms a reaction channel 8 between housing 6 and the inner casing 7, The diazo-reaction that is used for uncle's arylamine, the cavity 10 of inner casing 7 is used for passing into cooling medium;
One is arranged on the housing 6 outer cooling jackets 9 that are used for passing into cooling medium;
Feed(raw material)inlet 11 is arranged on reactor shell 6 bottoms, and reacting product outlet 12 is arranged on reactor enclosure The top of body 6.
Owing to adopted above-mentioned tubular reactor with dual-cooled, will greatly improve the heat transfer of reactor Efficient is avoided the too high and decomposition of the diazol that causes of local temperature.
Embodiment 1
The structural parameter of first tubular reactor 3:
The internal diameter of housing 6 is 35mm, and the external diameter of inner casing 7 is 25mm, and height for reactor is 3m;
The structural parameter of second tubular reactor 5:
The internal diameter of housing 6 is 35mm, and the external diameter of inner casing 7 is 25mm, and height for reactor is 2m;
Processing condition:
Temperature of reaction is 25 ℃, and the charge proportion of first tubular reactor is:
Uncle's arylamine: sulfuric acid: Sodium Nitrite=1: 4: 1.05;
The flow of uncle's arylamine and sulfuric acid mixed solution is 1200 kilograms/hour;
After replenishing Sodium Nitrite, the reaction product that flows out first tubular reactor enters second reactor 5, magnitude of recruitment is 30 kilograms/hour, synthetic diazonium salt of triarylamine solution flows out from the top of second reactor 5,50% refluxes, all the other enter follow-up workshop section as finished product, output is 1830 kilograms/hour, and weight percent content is 22%.
Claims (5)
1. the method for a continuously preparing diazonium salt of triarylamine, it is characterized in that, uncle's arylamine is continuously imported the bottom that have first tubular reactor (3) of cooling jacket by feedstock pump (1), sodium nitrite solution by nitrous acid sodium pump (2) with the mixing solutions of sulfuric acid or hydrochloric acid, reaction generates diazonium salt of triarylamine, flows out from the top of tubular reactor (3).
2. the method for claim 1, its feature also is, the reaction product that flows out first tubular reactor (3) top is cooled off, and is replenished the bottom that enters second reactor (5) that has cooling jacket behind the sodium nitrite solution again by water cooler (4), at last, synthetic diazonium salt of triarylamine solution flows out from the top of second reactor (5), partial reflux, mixing solutions, sodium nitrite solution with arylamine, sulfuric acid or hydrochloric acid enter first tubular reactor (3) again, and part enters follow-up workshop section as finished product.
3. method as claimed in claim 1 or 2 is characterized in that, temperature of reaction is generally 0～50 ℃; The charge proportion of first tubular reactor is:
Uncle's arylamine: sulfuric acid or hydrochloric acid: Sodium Nitrite=1: 1～8: 1～1.1;
The residence time of material in reactor is 0.5～60s.
4. one kind is used to realize the described device of claim 2, it is characterized in that this device comprises:
First tubular reactor (3) that has cooling jacket;
Second tubular reactor (5) that has cooling jacket, the outlet of this reactor is connected with the inlet of follow-up workshop section and first tubular reactor (3);
A water cooler (4) that is connected with first tubular reactor (3) top exit and second tubular reactor (5) bottom inlet respectively;
A feedstock pump (1) and a nitrous acid sodium pump (2) all are connected by the bottom inlet of pipeline with first reactor (3); Nitrous acid sodium pump (2) is connected by the inlet of pipeline with second reactor (5) bottom.
5. device as claimed in claim 4 is characterized in that, said reactor comprises:
A cylindrical shell (6);
One and the concentric inner casing of housing (6) (7) form a reaction channel (8) between housing (6) and the inner casing (7), inner casing (7) has the cavity (10) that is used to feed heat-eliminating medium;
One is arranged on the outer cooling jacket (9) that is used to feed heat-eliminating medium of housing (6);
Feed(raw material)inlet (11) is arranged on reactor shell (6) bottom, and reacting product outlet (12) is arranged on the top of reactor shell (6).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011052554A CN1162402C (en) | 2001-01-19 | 2001-01-19 | Process for equipment for continuously preparing diazonium salt of triarylamine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011052554A CN1162402C (en) | 2001-01-19 | 2001-01-19 | Process for equipment for continuously preparing diazonium salt of triarylamine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1365968A CN1365968A (en) | 2002-08-28 |
| CN1162402C true CN1162402C (en) | 2004-08-18 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011052554A Expired - Lifetime CN1162402C (en) | 2001-01-19 | 2001-01-19 | Process for equipment for continuously preparing diazonium salt of triarylamine |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103130679B (en) * | 2013-03-12 | 2014-03-26 | 浙江迪邦化工有限公司 | Method and device for automatic control continuous production of diazo compound |
| CN103263884B (en) * | 2013-06-08 | 2015-07-08 | 上海海唇机械设备工程技术有限公司 | Synthesis reactor and device and method for synthesizing methylhydrazine by chloramine process |
| CN105348847B (en) * | 2015-11-13 | 2017-10-10 | 浙江闰土研究院有限公司 | A kind of continuous coupling process of dyestuff |
| CN107857703B (en) * | 2017-09-14 | 2024-02-09 | 北京凯瑞英科技有限公司 | Reactor and method for continuously producing nitromethane |
| CN113527136B (en) * | 2021-08-19 | 2023-08-04 | 浙江迪邦化工有限公司 | System and process for producing diazonium salt of p-nitroaniline |
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2001
- 2001-01-19 CN CNB011052554A patent/CN1162402C/en not_active Expired - Lifetime
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| CN1365968A (en) | 2002-08-28 |
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Granted publication date: 20040818 |