CN102614680B - Caffeine crystallization method based on low energy consumption - Google Patents
Caffeine crystallization method based on low energy consumption Download PDFInfo
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- CN102614680B CN102614680B CN201210110809.0A CN201210110809A CN102614680B CN 102614680 B CN102614680 B CN 102614680B CN 201210110809 A CN201210110809 A CN 201210110809A CN 102614680 B CN102614680 B CN 102614680B
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- caffeine
- heat exchanger
- crystallization
- filtrate
- mother liquor
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- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 title claims abstract description 192
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 229960001948 caffeine Drugs 0.000 title claims abstract description 96
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 238000002425 crystallisation Methods 0.000 title claims abstract description 51
- 238000005265 energy consumption Methods 0.000 title abstract description 8
- 230000008025 crystallization Effects 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 33
- 239000012452 mother liquor Substances 0.000 claims abstract description 26
- 239000000498 cooling water Substances 0.000 claims abstract description 25
- 239000000706 filtrate Substances 0.000 claims description 33
- 239000013078 crystal Substances 0.000 claims description 12
- 239000002826 coolant Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000001640 fractional crystallisation Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 230000000737 periodic effect Effects 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 abstract 1
- 239000012267 brine Substances 0.000 description 4
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 4
- 230000011218 segmentation Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000002269 analeptic agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019658 bitter taste Nutrition 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002503 metabolic effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- -1 xanthine alkaloid compound Chemical class 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a caffeine crystallization method based on low energy consumption, which uses a storage tank, a flow pump, a heat exchanger and a filter device for pipe-type continuous crystallization of caffeine mother liquor. By means of subsections, kettle-type periodic crystallization is converted into pipe-type continuous crystallization, and the phenomenon of large power consumption caused by high-power mixing in a periodic crystallization process can be avoided. Meanwhile, the process can greatly reduces consumption of cooling water. Compared with the prior art, consumption of cooling water can be reduced by approximately 60%.
Description
Technical field
The present invention relates to a kind of crystallization technique of caffeine, be specifically related to a kind of caffeine method for crystallising based on low energy consumption.
Background technology
Caffeine is a kind of xanthine alkaloid compound, and sterling coffee is because of the powdered substance of white, strong bitter taste, and it is a kind of central nervous system stimulant, is also metabolic stimulant simultaneously, is medically having a very important role.At present the method for industrial normal employing autoclave periodic crystallisation is processed the caffeine in mother liquor, and caffeine crystallization produces crystal, then with centrifuge by the caffeine centrifugation in magma.It is cooling that temperature-fall period adopts water at low temperature to carry out, and along with the generation of crystal, can adhere to unavoidably brilliant dirt, thereby heat transfer coefficient is seriously reduced on heating surface, and temperature fall time extends.And because disposable crystallization content is larger, in crystallization kettle, powerful agitating device must be set.Therefore, kettle type crystallization process exists the shortcoming that consumption of cooling-water is large, energy consumption is high.In addition, this technique also exists the shortcomings such as equipment investment is high, floor space is large, manpower consumption is many.The defect existing based on kettle type crystallization process, need to develop that a kind of energy consumption is low, reduced investment, novel process that occupation of land is few.
Summary of the invention
The present invention overcomes the deficiencies in the prior art, the caffeine that a kind of energy consumption is low and economic benefit is higher method for crystallising is provided, described method is converted into tubular type continuous crystallisation by segmentation by autoclave periodic crystallisation, can avoid the phenomenon of a large amount of power consumptions that batch crystallization process causes because of high-power stirring, this technique can greatly reduce cooling water consumption simultaneously, compared with former technique, cooling water consumption can reduce by 60% left and right.
Technical scheme of the present invention is: a kind of caffeine method for crystallising based on low energy consumption, and described method utilizes storage tank, flow pump, heat exchanger and filter apparatus to carry out tubular type continuous crystallisation to caffeine mother liquor, and concrete steps are:
The first step is put into the caffeine mother liquor of a certain amount of 78～85 DEG C in storage tank, and wherein content of caffeine is 20%～25%, makes the mother liquor two-stage heat exchanger of once flowing through by flow pump, logical cooling water;
Second step, adds a certain amount of crystal seed at the entrance of secondary heat exchanger, regulates the flow velocity of cooling medium, makes caffeine crystallization in secondary heat exchanger, and secondary heat exchanger outlet temperature is 52～58 DEG C.
The 3rd step, the mother liquor with filter after to crystallization carries out Separation of Solid and Liquid, and filtrate enters storage tank, and in filtrate, the content of caffeine is 7%～10%.
The 4th step, make filtrate flow through the successively third level and fourth stage heat exchanger by flow pump, add a certain amount of crystal seed at the entrance of fourth stage heat exchanger, regulate equally the flow velocity of cooling medium to make caffeine crystallization in heat exchanger, heat exchanger outlet temperature is 20～25 DEG C.
The 5th step, with the caffeine after filter fractional crystallization, in final filtrate, the content of caffeine is 1.1%～2.0%, filtrate can be used as cooling water and carries out cooling to the first order and second level heat exchanger.
The 6th step, is dried processing to the caffeine product obtaining in step 3 and step 5, the pure caffeine that can obtain being dried.
The invention has the beneficial effects as follows:
A kind of method for crystallising of caffeine is provided, by segmentation, autoclave periodic crystallisation is converted into tubular type continuous crystallisation, can avoid the phenomenon of a large amount of power consumptions that batch crystallization process causes because of high-power stirring, this technique can greatly reduce cooling water consumption simultaneously, compared with former technique, cooling water consumption can reduce by 60% left and right, has important practical significance for the reduction of caffeine production cost and the expansion of production capacity.
Detailed description of the invention
Embodiment mono-
The caffeine mother liquor that is 23% for content, when treating capacity is 3m
3when/h, after one section of crystallization, obtain caffeine 345Kg, filtrate content is to obtain caffeine 225Kg after 12%, two section of crystallization, and filtrate content is 3%.Produce 1000Kg caffeine, cooling water consumption is 2500Kg, and the consumption of chilled brine is 5000Kg.
Embodiment bis-
The caffeine mother liquor that is 23% for content, when treating capacity is 5m
3when/h, after one section of crystallization, obtain caffeine 575Kg, filtrate content is to obtain caffeine 514Kg after 13%, two section of crystallization, and filtrate content is 3.5%.Produce 1000Kg caffeine, cooling water consumption is 5000Kg, and the consumption of chilled brine is 8000Kg.
Embodiment tri-
The caffeine mother liquor that is 23% for content, when treating capacity is 7m
3when/h, after one section of crystallization, obtain caffeine 840Kg, filtrate content is to obtain caffeine 716Kg after 12.5%, two section of crystallization, and filtrate content is 3%.Produce 1000Kg caffeine, cooling water consumption is 8500Kg, and the consumption of chilled brine is 11500Kg.
Embodiment tetra-
The caffeine mother liquor that is 23% for content, when treating capacity is 9m
3when/h, after one section of crystallization, obtain caffeine 1120Kg, filtrate content is to obtain caffeine 915Kg after 12%, two section of crystallization, and filtrate content is 2.5%.Produce 1000Kg caffeine, cooling water consumption is 11500Kg, and the consumption of chilled brine is 14000Kg.
Claims (4)
1. a method for caffeine tubular type continuous crystallisation, is characterized in that: described method utilizes storage tank, flow pump, heat exchanger and filter apparatus to carry out tubular type continuous crystallisation to caffeine mother liquor, and concrete steps are:
The first step is put into the caffeine mother liquor of 78～85 DEG C in storage tank, and wherein content of caffeine is 23%, makes the mother liquor two-stage heat exchanger of once flowing through by flow pump, logical cooling water;
Second step, adds a certain amount of crystal seed at the entrance of secondary heat exchanger, regulates the flow velocity of cooling medium, makes caffeine crystallization in secondary heat exchanger, and secondary heat exchanger outlet temperature is 52～58 DEG C;
The 3rd step, the mother liquor with filter after to crystallization carries out Separation of Solid and Liquid, and filtrate enters storage tank, and in filtrate, the content of caffeine is 12%;
The 4th step, make filtrate flow through the successively third level and fourth stage heat exchanger by flow pump, add a certain amount of crystal seed at the entrance of fourth stage heat exchanger, regulate equally the flow velocity of cooling medium to make caffeine crystallization in heat exchanger, heat exchanger outlet temperature is 20～25 DEG C;
The 5th step, with the caffeine after filter fractional crystallization, in final filtrate, the content of caffeine is 3%, uses final filtrate to carry out cooling as cooling water to the first order and second level heat exchanger;
Wherein the caffeine product obtaining in step 3 is dried to processing, the pure caffeine that can obtain being dried;
The caffeine obtaining in step 5 is dried to processing, the pure caffeine that also can obtain being dried;
The method can reduce power consumption and the power consumption energy of cooling water, reduces caffeine production cost.
2. a method for caffeine tubular type continuous crystallisation, is characterized in that: described method utilizes storage tank, flow pump, heat exchanger and filter apparatus to carry out tubular type continuous crystallisation to caffeine mother liquor, and concrete steps are:
The first step is put into the caffeine mother liquor of 78～85 DEG C in storage tank, and wherein content of caffeine is 23%, makes the mother liquor two-stage heat exchanger of once flowing through by flow pump, logical cooling water;
Second step, adds a certain amount of crystal seed at the entrance of secondary heat exchanger, regulates the flow velocity of cooling medium, makes caffeine crystallization in secondary heat exchanger, and secondary heat exchanger outlet temperature is 52～58 DEG C;
The 3rd step, the mother liquor with filter after to crystallization carries out Separation of Solid and Liquid, and filtrate enters storage tank, and in filtrate, the content of caffeine is 13%;
The 4th step, make filtrate flow through the successively third level and fourth stage heat exchanger by flow pump, add a certain amount of crystal seed at the entrance of fourth stage heat exchanger, regulate equally the flow velocity of cooling medium to make caffeine crystallization in heat exchanger, heat exchanger outlet temperature is 20～25 DEG C;
The 5th step, with the caffeine after filter fractional crystallization, in final filtrate, the content of caffeine is 3.5%, uses final filtrate to carry out cooling as cooling water to the first order and second level heat exchanger;
Wherein the caffeine product obtaining in step 3 is dried to processing, the pure caffeine that can obtain being dried;
The caffeine obtaining in step 5 is dried to processing, the pure caffeine that also can obtain being dried;
The method can reduce power consumption and the power consumption energy of cooling water, reduces caffeine production cost.
3. a method for caffeine tubular type continuous crystallisation, is characterized in that: described method utilizes storage tank, flow pump, heat exchanger and filter apparatus to carry out tubular type continuous crystallisation to caffeine mother liquor, and concrete steps are:
The first step is put into the caffeine mother liquor of 78～85 DEG C in storage tank, and wherein content of caffeine is 23%, makes the mother liquor two-stage heat exchanger of once flowing through by flow pump, logical cooling water;
Second step, adds a certain amount of crystal seed at the entrance of secondary heat exchanger, regulates the flow velocity of cooling medium, makes caffeine crystallization in secondary heat exchanger, and secondary heat exchanger outlet temperature is 52～58 DEG C;
The 3rd step, the mother liquor with filter after to crystallization carries out Separation of Solid and Liquid, and filtrate enters storage tank, and in filtrate, the content of caffeine is 12.5%;
The 4th step, make filtrate flow through the successively third level and fourth stage heat exchanger by flow pump, add a certain amount of crystal seed at the entrance of fourth stage heat exchanger, regulate equally the flow velocity of cooling medium to make caffeine crystallization in heat exchanger, heat exchanger outlet temperature is 20～25 DEG C;
The 5th step, with the caffeine after filter fractional crystallization, in final filtrate, the content of caffeine is 3.0%, uses final filtrate to carry out cooling as cooling water to the first order and second level heat exchanger;
Wherein the caffeine product obtaining in step 3 is dried to processing, the pure caffeine that can obtain being dried;
The caffeine obtaining in step 5 is dried to processing, the pure caffeine that also can obtain being dried;
The method can reduce power consumption and the power consumption energy of cooling water, reduces caffeine production cost.
4. a method for caffeine tubular type continuous crystallisation, is characterized in that: described method utilizes storage tank, flow pump, heat exchanger and filter apparatus to carry out tubular type continuous crystallisation to caffeine mother liquor, and concrete steps are:
The first step is put into the caffeine mother liquor of 78～85 DEG C in storage tank, and wherein content of caffeine is 23%, makes the mother liquor two-stage heat exchanger of once flowing through by flow pump, logical cooling water;
Second step, adds a certain amount of crystal seed at the entrance of secondary heat exchanger, regulates the flow velocity of cooling medium, makes caffeine crystallization in secondary heat exchanger, and secondary heat exchanger outlet temperature is 52～58 DEG C;
The 3rd step, the mother liquor with filter after to crystallization carries out Separation of Solid and Liquid, and filtrate enters storage tank, and in filtrate, the content of caffeine is 12%;
The 4th step, make filtrate flow through the successively third level and fourth stage heat exchanger by flow pump, add a certain amount of crystal seed at the entrance of fourth stage heat exchanger, regulate equally the flow velocity of cooling medium to make caffeine crystallization in heat exchanger, heat exchanger outlet temperature is 20～25 DEG C;
The 5th step, with the caffeine after filter fractional crystallization, in final filtrate, the content of caffeine is 2.5%, uses final filtrate to carry out cooling as cooling water to the first order and second level heat exchanger;
Wherein the caffeine product obtaining in step 3 is dried to processing, the pure caffeine that can obtain being dried;
The caffeine obtaining in step 5 is dried to processing, the pure caffeine that also can obtain being dried;
The method can reduce power consumption and the power consumption energy of cooling water, reduces caffeine production cost.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210110809.0A CN102614680B (en) | 2012-04-16 | 2012-04-16 | Caffeine crystallization method based on low energy consumption |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210110809.0A CN102614680B (en) | 2012-04-16 | 2012-04-16 | Caffeine crystallization method based on low energy consumption |
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| CN102614680A CN102614680A (en) | 2012-08-01 |
| CN102614680B true CN102614680B (en) | 2014-09-10 |
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| CN103980276A (en) * | 2014-05-26 | 2014-08-13 | 中国药科大学 | Quercetin caffeine eutectic |
| CN110052075A (en) * | 2019-06-05 | 2019-07-26 | 太仓塑料助剂厂有限公司 | The separation method and system of cumyl peroxide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3530924A (en) * | 1967-03-03 | 1970-09-29 | Wintershall Ag | Crystallization method and device |
| US3722229A (en) * | 1970-12-29 | 1973-03-27 | Maruzen Oil Co Ltd | Smooth surface chiller crystallizer |
| CN1958112A (en) * | 2006-10-20 | 2007-05-09 | 西安航天华威化工生物工程有限公司 | Equipment of crystallisation by cooling, and cooling method |
-
2012
- 2012-04-16 CN CN201210110809.0A patent/CN102614680B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3530924A (en) * | 1967-03-03 | 1970-09-29 | Wintershall Ag | Crystallization method and device |
| US3722229A (en) * | 1970-12-29 | 1973-03-27 | Maruzen Oil Co Ltd | Smooth surface chiller crystallizer |
| CN1958112A (en) * | 2006-10-20 | 2007-05-09 | 西安航天华威化工生物工程有限公司 | Equipment of crystallisation by cooling, and cooling method |
Non-Patent Citations (1)
| Title |
|---|
| 朱兆友，张大卫，.咖啡因分段结晶工艺研究.《化学与生物工程》.2011,第28卷(第12期),第2页第1段、第2页最后一段、第3页第3段、附图3及表1-2. * |
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