CN103044265A - Device and method for producing high-concentration trimethylamine hydrochloride - Google Patents
Device and method for producing high-concentration trimethylamine hydrochloride Download PDFInfo
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- CN103044265A CN103044265A CN2012105634803A CN201210563480A CN103044265A CN 103044265 A CN103044265 A CN 103044265A CN 2012105634803 A CN2012105634803 A CN 2012105634803A CN 201210563480 A CN201210563480 A CN 201210563480A CN 103044265 A CN103044265 A CN 103044265A
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- hydrochloric acid
- hydrogen chloride
- trimethylamine
- trimethylamine hydrochloride
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Abstract
The invention discloses a device for producing high-concentration trimethylamine hydrochloride, which comprises a hydrochloric acid concentration absorber, a hydrochloric acid concentration adsorption tank, a primary reactor, a hydrogen chloride absorber, a hydrogen chloride adsorption tank, a secondary reactor and a salt forming vessel. The invention also discloses a method for producing the high-concentration trimethylamine hydrochloride, which comprises the following steps of: firstly, circulating and concentrating hydrochloric acid and hydrogen chloride in the hydrochloric acid concentration absorber and the hydrochloric acid concentration adsorption tank, then entering into the primary reactor, reacting with trimethylamine, entering the hydrogen chloride absorber after reaction, circulating the trimethylamine hydrochloride and the hydrogen chloride between the hydrogen chloride absorber and the hydrogen chloride adsorption tank, then entering the secondary reactor, reacting with the trimethylamine, conveying into the salt forming vessel after reaction and outputting. By utilizing the device and the method, the high-concentration trimethylamine hydrochloride (which can reach 67-70 percent) can be produced, the steps are simple, the cost is low, and the production of a downstream choline chloride product is facilitated, therefore, the device and the method can be popularized and applied.
Description
Technical field
The present invention relates to a kind of device and method of producing the high density trimethylamine hydrochloride, belong to the Chemicals production field.
Background technology
At present, trimethylamine hydrochloride production generally adopts 31% technical hydrochloric acid and 99.7～99.8% Trimethylamine 99 to react, and output concentration is 53%～54% trimethylamine hydrochloride solution, is directly used in feed additive industry and produces choline chloride 60.But 53%～54% trimethylamine hydrochloride is directly used in the production of choline chloride 60, and the choline chloride solution degree of output is 62%～63%, and concentration is low, and manufacturing enterprise need to carry out further evaporation concentration with the concentration of raising the finished product, complex steps, and cost is higher.If can directly adopt the trimethylamine hydrochloride of higher concentration to produce choline chloride 60, then can reduce the concentrated process of choline chloride 60, even just can directly not obtain to expect the choline chloride 60 product of concentration with evaporation concentration.In the prior art and have no report relevant for the trimethylamine hydrochloride of production high density.
Summary of the invention
For above-mentioned prior art, the invention provides a kind of device of producing the high density trimethylamine hydrochloride, and the method for production high density trimethylamine hydrochloride.
The present invention is achieved by the following technical solutions:
A kind of device of producing the high density trimethylamine hydrochloride, comprise hydrochloric acid concentrate resorber, hydrochloric acid concentrate absorption cell, A reactor, hydrogen chloride absorption device, hydrogen chloride absorption groove, second reactor and become salt oven, wherein, hydrochloric acid concentrate absorber bottom is connected with hydrochloric acid concentrate absorption cell top; Be connected with A reactor with hydrochloric acid concentrate absorber overhead respectively and be connected in hydrochloric acid concentrate absorption cell bottom, connecting pipeline is provided with recycle pump and control valve; The A reactor top is connected with hydrogen chloride absorption device top; Hydrogen chloride absorption device bottom is connected with hydrogen chloride absorption groove top; The hydrogen chloride absorption trench bottom is connected with second reactor with hydrogen chloride absorption device top respectively and is connected, and connecting pipeline is provided with recycle pump and control valve; The second reactor top is connected with becoming the salt oven top; Become between salt oven top and the bottom to be provided with circulation line, circulation line is provided with recycle pump and trimethylamine hydrochloride finished product pipeline; Hydrochloric acid concentrate absorber overhead and hydrogen chloride absorption device top all are connected with the hydrogen chloride gas pipeline; Hydrochloric acid concentrate absorber overhead is connected with the hydrochloric acid pipeline; All be connected with the tail gas recycle pipeline on hydrochloric acid concentrate absorption cell and the hydrogen chloride absorption groove; A reactor and second reactor bottom all are connected with the Trimethylamine 99 pipeline; Described connection is pipeline and connects.
Described one-tenth salt oven top is connected with hydrochloric acid pipeline and Trimethylamine 99 pipeline.
Described hydrochloric acid concentrate resorber is graphite heat exchanger, and heat-eliminating medium is recirculated water, and specification is ￠ 620 * 5240, and heat interchanging area is 60m
2, the access arrangement concentration of hydrochloric acid is 31%, and the transport pipe nominal diameter is DN50, and hydrogenchloride purity is 95～96%, and the transport pipe nominal diameter is DN200, concentration of hydrochloric acid increases to 34～35% after concentrate.
Described A reactor is graphite heat exchanger, and heat-eliminating medium is recirculated water, and specification is ￠ 886 * 6564, and heat interchanging area is 120m
2, the access arrangement concentration of hydrochloric acid is 34～35%, Trimethylamine 99 purity is 99.7～99.8%, and the transport pipe nominal diameter is DN50, and control pressure is at＜0.2MPa, and trimethylamine hydrochloride concentration increases to 57～58.6% after concentrate.
Described hydrogen chloride absorption device is graphite heat exchanger, and heat-eliminating medium is recirculated water, and specification is ￠ 620 * 5240, and heat interchanging area is 60m
2, access arrangement Trimethylamine 99 concentration of hydrochloric acid is 57～58.6%, and the transport pipe nominal diameter is DN65, and hydrogenchloride purity is 95～96%, and the transport pipe nominal diameter is DN200, trimethylamine hydrochloride pH value reaches 1～2 after absorbing.
Described second reactor is graphite heat exchanger, and heat-eliminating medium is recirculated water, and specification is ￠ 886 * 6564, and heat interchanging area is 120m
2, access arrangement trimethylamine hydrochloride pH value 1～2, Trimethylamine 99 purity is 99.7～99.8%, and the transport pipe nominal diameter is DN50, and control pressure is at＜0.2MPa, and trimethylamine hydrochloride concentration increases to 67～70% after concentrate.
Described hydrochloric acid concentrate absorption cell, hydrogen chloride absorption groove material are glass reinforced plastic, and specification is ￠ 1350 * 2100, and volume is 3.7m
2
Described one-tenth salt oven is jacketed lass lining enclosed reactor, housing parameter: use temperature: 100 ℃; Chuck parameter: media name: recirculated cooling water, use temperature :≤60, volume 8m
3
Described recycle pump is magnetic drive pump, flow: 30m
3∕ h, lift: 20m.
A kind of method of producing the high density trimethylamine hydrochloride, step is as follows: at first, 31% hydrochloric acid and 95～96% hydrogenchloride are at hydrochloric acid concentrate resorber, juice circulation between the hydrochloric acid concentrate absorption cell, when treating that concentration of hydrochloric acid increases to 34～35%, enter A reactor, with purity be that 99.7～99.8% Trimethylamine 99 reacts, reacted trimethylamine hydrochloride (trimethylamine hydrochloride concentration is 57～58.6%) enters the hydrogen chloride absorption device, trimethylamine hydrochloride and hydrogenchloride are at the hydrogen chloride absorption device, circulate between the hydrogen chloride absorption groove, the abundant absorbing hydrogen chloride of trimethylamine hydrochloride, reduce the pH value, treat that trimethylamine hydrochloride pH value was down at 1～2 o'clock, enter second reactor, with concentration be that 99.7～99.8% Trimethylamine 99 reacts, after the reaction, trimethylamine hydrochloride concentration can reach 67～70%, send into into salt oven, then trimethylamine hydrochloride is by the output of trimethylamine hydrochloride finished product pipeline, and the tail gas of generation is sent into tail gas absorption tank by the tail gas recycle pipeline and reclaimed.
After described trimethylamine hydrochloride enters into salt oven, for guaranteeing qualified product, can in the one-tenth salt oven, add micro-Trimethylamine 99 or/and the salt acid for adjusting pH value is adjusted to required pH(such as pH6.5～7).
Percentage ratio described above is mass percent.
Utilize apparatus and method of the present invention can produce the trimethylamine hydrochloride of high density, step is simple, and is with low cost, and the concentration of trimethylamine hydrochloride product can reach 67～70%.Production method of the present invention, improved the concentration of trimethylamine hydrochloride, make things convenient for the production of downstream choline chloride 60 product (to save the evaporation link, steam saving, but produce choline chloride 60 steam saving 200Kg per ton, shorten to produce simultaneously the choline chloride 60 technical process), can also reduce the costs of transportation and management of unit product, cost is low, can apply.
Description of drawings
Fig. 1 is the structural representation of the device of production high density trimethylamine hydrochloride of the present invention.
Fig. 2 is the process flow sheet (arrow is depicted as the flow direction of material in the pipeline among the figure) of the method for production high density trimethylamine hydrochloride of the present invention.
Wherein, 1, hydrochloric acid concentrate resorber; 2, hydrochloric acid concentrate absorption cell; 3, A reactor; 4, hydrogen chloride absorption device; 5, hydrogen chloride absorption groove; 6, second reactor; 7, become salt oven; 8, recycle pump;
A, hydrogen chloride gas pipeline; B, hydrochloric acid pipeline; C, circulation water inlet; The D circulating backwater; E, 34～35% hydrochloric acid; F, Trimethylamine 99 pipeline; G, 57～58.6% trimethylamine hydrochlorides; The trimethylamine hydrochloride of H, pH1～2; I, 67～70% trimethylamine hydrochloride; J, trimethylamine hydrochloride finished product pipeline; K, tail gas recycle pipeline.
Embodiment
The present invention is further illustrated below in conjunction with drawings and Examples.
Embodiment 1
A kind of device of producing the high density trimethylamine hydrochloride, comprise hydrochloric acid concentrate resorber 1, hydrochloric acid concentrate absorption cell 2, A reactor 3, hydrogen chloride absorption device 4, hydrogen chloride absorption groove 5, second reactor 6 and become salt oven 7, as shown in Figure 1, wherein, hydrochloric acid concentrate resorber 1 bottom is connected with hydrochloric acid concentrate absorption cell 2 tops; Are connected the bottom with hydrochloric acid concentrate resorber 1 top respectively and are connected in hydrochloric acid concentrate absorption cell 2 bottoms with A reactor, connecting pipeline is provided with recycle pump 8 and control valve; A reactor 3 tops are connected with hydrogen chloride absorption device 4 tops; Hydrogen chloride absorption device 4 bottoms are connected with hydrogen chloride absorption groove 5 tops; Are connected the bottom with hydrogen chloride absorption device 4 tops respectively and are connected in hydrogen chloride absorption groove 5 bottoms with second reactor, connecting pipeline is provided with recycle pump 8 and control valve; Second reactor 6 tops are connected with becoming salt oven 7 tops; Become between salt oven 7 tops and the bottom to be provided with circulation line, circulation line is provided with recycle pump 8 and trimethylamine hydrochloride finished product pipeline J; Hydrochloric acid concentrate resorber 1 top and hydrogen chloride absorption device 4 tops all are connected with hydrogen chloride gas pipeline A; Hydrochloric acid concentrate resorber 1 top is connected with hydrochloric acid pipeline B; All be connected with tail gas recycle pipeline K on hydrochloric acid concentrate absorption cell 2 and the hydrogen chloride absorption groove 5; A reactor 3 and second reactor 6 bottoms all are connected with Trimethylamine 99 pipeline F; Become salt oven 7 tops to be connected with hydrochloric acid pipeline B and Trimethylamine 99 pipeline F; Described connection is pipeline and connects.
Utilize the method for said apparatus production high density trimethylamine hydrochloride, schema as shown in Figure 2, step is as follows: at first, 31% hydrochloric acid (carrying by hydrochloric acid pipeline B) and 95～96% hydrogenchloride (carrying by hydrogen chloride gas pipeline A) are at hydrochloric acid concentrate resorber 1, juice circulation between the hydrochloric acid concentrate absorption cell 2, treat that concentration of hydrochloric acid increases among 34～35%(Fig. 2 shown in the E) time, enter A reactor 3, with purity be that 99.7～99.8% Trimethylamine 99 (carrying by Trimethylamine 99 pipeline F) reacts, (trimethylamine hydrochloride concentration is 57～58.6% for reacted trimethylamine hydrochloride, among Fig. 2 shown in the G) enter hydrogen chloride absorption device 4, trimethylamine hydrochloride and hydrogenchloride (carrying by hydrogen chloride gas pipeline A) are at hydrogen chloride absorption device 4, circulation between the hydrogen chloride absorption groove 5, the abundant absorbing hydrogen chloride of trimethylamine hydrochloride, reduce the pH value, treat that trimethylamine hydrochloride pH value is down among 1～2(Fig. 2 shown in the H) time, enter second reactor 6, with concentration be that 99.7～99.8% Trimethylamine 99 (carrying by Trimethylamine 99 pipeline F) reacts, after the reaction, trimethylamine hydrochloride concentration can reach among 67～70%(Fig. 2 shown in the I), send into into salt oven 7, for guaranteeing qualified product, to becoming to add in the salt oven micro-Trimethylamine 99 (carrying by Trimethylamine 99 pipeline F) or/and hydrochloric acid (carrying by hydrochloric acid pipeline B) is regulated the pH value, be adjusted to required pH6.5～7, then trimethylamine hydrochloride is by trimethylamine hydrochloride finished product pipeline J output, and the tail gas of generation is sent into tail gas absorption tank by tail gas recycle pipeline K and reclaimed.
Described hydrochloric acid concentrate resorber is graphite heat exchanger, and heat-eliminating medium is recirculated water (recirculated water refluxes by circulation water inlet C and circulating backwater D), and specification is ￠ 620 * 5240, and heat interchanging area is 60m
2, the access arrangement concentration of hydrochloric acid is 31%, and the transport pipe nominal diameter is DN50, and hydrogenchloride purity is 95～96%, and the transport pipe nominal diameter is DN200, concentration of hydrochloric acid increases to 34～35% after concentrate.
Described A reactor is graphite heat exchanger, and heat-eliminating medium is recirculated water, and specification is ￠ 886 * 6564, and heat interchanging area is 120m
2, the access arrangement concentration of hydrochloric acid is 34～35%, Trimethylamine 99 purity is 99.7～99.8%, and the transport pipe nominal diameter is DN50, and control pressure is at＜0.2MPa, and trimethylamine hydrochloride concentration increases to 57～58.6% after concentrate.
Described hydrogen chloride absorption device is graphite heat exchanger, and heat-eliminating medium is recirculated water, and specification is ￠ 620 * 5240, and heat interchanging area is 60m
2, access arrangement Trimethylamine 99 concentration of hydrochloric acid is 57～58.6%, and the transport pipe nominal diameter is DN65, and hydrogenchloride purity is 95～96%, and the transport pipe nominal diameter is DN200, trimethylamine hydrochloride pH value reaches 1～2 after absorbing.
Described second reactor is graphite heat exchanger, and heat-eliminating medium is recirculated water, and specification is ￠ 886 * 6564, and heat interchanging area is 120m
2, access arrangement trimethylamine hydrochloride pH value 1～2, Trimethylamine 99 purity is 99.7～99.8%, and the transport pipe nominal diameter is DN50, and control pressure is at＜0.2MPa, and trimethylamine hydrochloride concentration increases to 67～70% after concentrate.
Described hydrochloric acid concentrate absorption cell, hydrogen chloride absorption groove material are glass reinforced plastic, and specification is ￠ 1350 * 2100, and volume is 3.7m
2
Described one-tenth salt oven is jacketed lass lining enclosed reactor, housing parameter: use temperature: 100 ℃; Chuck parameter: media name: recirculated cooling water, use temperature :≤60, volume 8m
3
Described recycle pump is magnetic drive pump, flow: 30m
3∕ h, lift: 20m.
Claims (10)
1. device of producing the high density trimethylamine hydrochloride, it is characterized in that: comprise hydrochloric acid concentrate resorber, hydrochloric acid concentrate absorption cell, A reactor, hydrogen chloride absorption device, hydrogen chloride absorption groove, second reactor and become salt oven, wherein, hydrochloric acid concentrate absorber bottom is connected with hydrochloric acid concentrate absorption cell top; Be connected with A reactor with hydrochloric acid concentrate absorber overhead respectively and be connected in hydrochloric acid concentrate absorption cell bottom, connecting pipeline is provided with recycle pump and control valve; The A reactor top is connected with hydrogen chloride absorption device top; Hydrogen chloride absorption device bottom is connected with hydrogen chloride absorption groove top; The hydrogen chloride absorption trench bottom is connected with second reactor with hydrogen chloride absorption device top respectively and is connected, and connecting pipeline is provided with recycle pump and control valve; The second reactor top is connected with becoming the salt oven top; Become between salt oven top and the bottom to be provided with circulation line, circulation line is provided with recycle pump and trimethylamine hydrochloride finished product pipeline; Hydrochloric acid concentrate absorber overhead and hydrogen chloride absorption device top all are connected with the hydrogen chloride gas pipeline; Hydrochloric acid concentrate absorber overhead is connected with the hydrochloric acid pipeline; All be connected with the tail gas recycle pipeline on hydrochloric acid concentrate absorption cell and the hydrogen chloride absorption groove; A reactor and second reactor bottom all are connected with the Trimethylamine 99 pipeline; Described connection is pipeline and connects.
2. a kind of device of producing the high density trimethylamine hydrochloride according to claim 1, it is characterized in that: described one-tenth salt oven top is connected with hydrochloric acid pipeline and Trimethylamine 99 pipeline.
3. a kind of device of producing the high density trimethylamine hydrochloride according to claim 1 and 2, it is characterized in that: described hydrochloric acid concentrate resorber is graphite heat exchanger, and heat-eliminating medium is recirculated water, and specification is ￠ 620 * 5240, and heat interchanging area is 60m
2
4. a kind of device of producing the high density trimethylamine hydrochloride according to claim 1 and 2, it is characterized in that: described A reactor is graphite heat exchanger, and heat-eliminating medium is recirculated water, and specification is ￠ 886 * 6564, and heat interchanging area is 120m
2
5. a kind of device of producing the high density trimethylamine hydrochloride according to claim 1 and 2, it is characterized in that: described hydrogen chloride absorption device is graphite heat exchanger, and heat-eliminating medium is recirculated water, and specification is ￠ 620 * 5240, and heat interchanging area is 60m
2
6. a kind of device of producing the high density trimethylamine hydrochloride according to claim 1 and 2, it is characterized in that: described second reactor is graphite heat exchanger, and heat-eliminating medium is recirculated water, and specification is ￠ 886 * 6564, and heat interchanging area is 120m
2
7. a kind of device of producing the high density trimethylamine hydrochloride according to claim 1 and 2, it is characterized in that: described hydrochloric acid concentrate absorption cell, hydrogen chloride absorption groove material are glass reinforced plastic, and specification is ￠ 1350 * 2100, and volume is 3.7m
2
8. a kind of device of producing the high density trimethylamine hydrochloride according to claim 1 and 2, it is characterized in that: described one-tenth salt oven is jacketed lass lining enclosed reactor, housing parameter: use temperature: 100 ℃; Chuck parameter: media name: recirculated cooling water, use temperature :≤60, volume 8m
3
9. method of producing the high density trimethylamine hydrochloride, it is characterized in that: step is as follows: at first, 31% hydrochloric acid and 95～96% hydrogenchloride are at hydrochloric acid concentrate resorber, juice circulation between the hydrochloric acid concentrate absorption cell, when treating that concentration of hydrochloric acid increases to 34～35%, enter A reactor, with purity be that 99.7～99.8% Trimethylamine 99 reacts, reacted trimethylamine hydrochloride enters the hydrogen chloride absorption device, trimethylamine hydrochloride and hydrogenchloride are at the hydrogen chloride absorption device, circulate between the hydrogen chloride absorption groove, treat that trimethylamine hydrochloride pH value was down at 1～2 o'clock, enter second reactor, with concentration be that 99.7～99.8% Trimethylamine 99 reacts, after the reaction, trimethylamine hydrochloride is sent into into salt oven, then trimethylamine hydrochloride is by the output of trimethylamine hydrochloride finished product pipeline, and the tail gas of generation is sent into tail gas absorption tank by the tail gas recycle pipeline and reclaimed.
10. a kind of method of producing the high density trimethylamine hydrochloride according to claim 9 is characterized in that: after described trimethylamine hydrochloride enters into salt oven, to becoming to add in the salt oven micro-Trimethylamine 99 or/and the salt acid for adjusting pH value is adjusted to pHpH6.5～7.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210563480.3A CN103044265B (en) | 2012-12-21 | 2012-12-21 | Device and method for producing high-concentration trimethylamine hydrochloride |
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|---|---|---|---|
| CN201210563480.3A CN103044265B (en) | 2012-12-21 | 2012-12-21 | Device and method for producing high-concentration trimethylamine hydrochloride |
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| CN103044265A true CN103044265A (en) | 2013-04-17 |
| CN103044265B CN103044265B (en) | 2014-04-23 |
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| CN201210563480.3A Expired - Fee Related CN103044265B (en) | 2012-12-21 | 2012-12-21 | Device and method for producing high-concentration trimethylamine hydrochloride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106560467A (en) * | 2016-06-27 | 2017-04-12 | 宁夏海诚电化信息科技有限公司 | Trimethylamine hydrochloride production process |
| CN115636751A (en) * | 2022-06-14 | 2023-01-24 | 山东一飞药业股份有限公司 | Production process of trimethylamine hydrochloride |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3872170A (en) * | 1971-03-29 | 1975-03-18 | Basf Ag | Continuous manufacture of an aqueous choline chloride solution |
| DD241595A1 (en) * | 1985-10-04 | 1986-12-17 | Chemisch Pharmazeutisches Werk | METHOD AND DEVICE FOR PREPARING CHOLIN CHLORIDE |
| CN101691333A (en) * | 2009-10-21 | 2010-04-07 | 山东恩贝科技有限公司 | Production technology for choline chloride |
-
2012
- 2012-12-21 CN CN201210563480.3A patent/CN103044265B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3872170A (en) * | 1971-03-29 | 1975-03-18 | Basf Ag | Continuous manufacture of an aqueous choline chloride solution |
| DD241595A1 (en) * | 1985-10-04 | 1986-12-17 | Chemisch Pharmazeutisches Werk | METHOD AND DEVICE FOR PREPARING CHOLIN CHLORIDE |
| CN101691333A (en) * | 2009-10-21 | 2010-04-07 | 山东恩贝科技有限公司 | Production technology for choline chloride |
Non-Patent Citations (1)
| Title |
|---|
| 刘晋，岳景娟，周威，徐玉洁: "合成氯化胆碱新工艺的研究", 《沈阳化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106560467A (en) * | 2016-06-27 | 2017-04-12 | 宁夏海诚电化信息科技有限公司 | Trimethylamine hydrochloride production process |
| CN115636751A (en) * | 2022-06-14 | 2023-01-24 | 山东一飞药业股份有限公司 | Production process of trimethylamine hydrochloride |
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| CN103044265B (en) | 2014-04-23 |
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