CN107353235A - A kind of evaporative crystallisation process of ox sulphur - Google Patents
A kind of evaporative crystallisation process of ox sulphur Download PDFInfo
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- CN107353235A CN107353235A CN201710576241.4A CN201710576241A CN107353235A CN 107353235 A CN107353235 A CN 107353235A CN 201710576241 A CN201710576241 A CN 201710576241A CN 107353235 A CN107353235 A CN 107353235A
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- magma
- taurine
- temperature
- sulphur
- concentrate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/42—Separation; Purification; Stabilisation; Use of additives
- C07C303/44—Separation; Purification
Abstract
The present invention discloses a kind of evaporative crystallisation process of ox sulphur, after taurine solution is heated, carries out refined filtration processing, obtains refined filtration liquid；Refined filtration liquid is concentrated by evaporation, obtains concentrate；After concentrate concentration reaches 32~35%, evaporative crystallization in crystallizing evaporator is delivered to, when concentration reaches 38~40%, stop into concentrate, it is 55~65 DEG C to control temperature, and 5000g crystal seeds are added into crystallizing evaporator, insulation 30~60 minutes, then slowly enter concentrate until recovering to 8m3/ h, at the same control temperature be 55~65 DEG C, backward crystallizing evaporator in it is secondary enter concentrate；After the solid-to-liquid ratio of magma reaches 40~50%, magma continuous discharge is carried out, the magma growing the grain of outflow is centrifuged and dried after 30~60 minutes, obtains ox sulphur crystal.This method technological process is simple, and crystallization process is easily-controllable, and the taurine crystal shape of gained has larger improvement compared with decrease temperature crystalline, is easy to later stage centrifugation, drying, storage, and prevented from caking.
Description
Technical field
The invention belongs to economic chemical technology field, specifically a kind of evaporative crystallisation process of ox sulphur.
Background technology
Taurine crystallization is realized by one-pot, single batch of charging, the mode intermittently operated of decrease temperature crystalline at present.Pass through
Circulated refrigerated water is passed through into crystallization kettle chuck to cool to 20~25 DEG C, reduces the solubility of ox sulphur, makes ox sulphur brilliant
Body separates out, and is then centrifuged, and the wet crystal after separation enters drying, and the mother liquor after separation concentrates again into concentration systems
Extraction.This decrease temperature crystalline method has the disadvantages that：Taurine is by decrease temperature crystalline, and crystal structure is in needle-like, easy fracture, no
Beneficial to later stage separation, drying and storage；Crystallization kettle single batch Batch Process, to reach certain production capacity, it is necessary to increase crystallization kettle
Quantity, causes that equipment is excessive, investment is larger；Every crystallization kettle will be controlled individually, and control point is more, temperature-fall period control difficulty compared with
Greatly；The mother liquor that decrease temperature crystalline is centrifuged out, concentration is relatively low, such as needs again purification to separate, then will produce a large amount of waste water, environmental protection treatment
Investment is big, and environmental risk is high.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of evaporative crystallisation process of ox sulphur, this method technological process
Simply, crystallization process is easily-controllable, and the taurine crystal shape of gained has larger improvement compared with decrease temperature crystalline, be easy to the later stage centrifugation, drying,
Storage, it is prevented from caking, and substantially reduce the generation of waste water in production process.
In order to solve the above technical problems, the invention provides a kind of evaporative crystallisation process of ox sulphur, comprise the following steps：
(1) after the taurine solution that concentration is 20~25% being heated into 60~80 DEG C, carried out by fine filter at refined filtration
Reason, impurity in solution is removed, obtains taurine refined filtration liquid；
(2) taurine refined filtration liquid is delivered into evaporation concentrator, the feed rate for controlling taurine refined filtration liquid is 12m3/ h, steaming
Hair thickening temperature is 75~80 DEG C, vacuum is -50~-69KPa in evaporation concentrator, is evaporated concentration, obtains concentrate；
(3) after concentrate concentration reaches 32%~35%, deliver in crystallizing evaporator, control the feed rate of concentrate
For 8m3/ h, evaporative crystallization temperature are 55~65 DEG C, are evaporated crystallization, when concentration reaches 38%~40%, in crystallizing evaporator
Material reaches hypersaturated state, now stops charging, while it is 55~65 DEG C to control temperature, by crystal seed tank to crystallizing evaporator
Middle addition 5000g taurine crystal seeds, and 30~60 minutes are incubated, slowly enter concentrate afterwards until recovering to 8m3/ h, same to time control
Temperature processed is 55~65 DEG C and is evaporated crystallization；
(4) after the solid-to-liquid ratio of magma in crystallizing evaporator reaches 40~50%, magma continuous discharge, magma are carried out
Liquid discharging flow is 5~6m3/ h, the magma of outflow are sent into maturator, control maturator temperature and magma drop temperature
The temperature difference balances each other, growing the grain 30~60 minutes；
(5) magma after growing the grain delivers to centrifuge and carries out continuous centrifugal separation, the taurine wet crystal after centrifugation
It is dried into dryer, you can obtain dry ox sulphur crystal.
Present invention process is simple, does not need large batch of monomer crystallization kettle especially, reduces equipment investment and workshop building
Investment；Evaporation and crystal process is continuous production, and control point is few, easily realizes Automated condtrol, and the stability of production greatly improves；
The taurine crystal grain of gained of the invention is uniform compared with the taurine crystal structure that decrease temperature crystalline obtains, and consistency is high, after being easy to
Phase centrifugation, drying, not easy to break, finished product is prevented from caking, is readily transported and stores.
Brief description of the drawings
Fig. 1 is the process chart of the evaporative crystallisation process of ox sulphur of the present invention.
Embodiment
Below in conjunction with the embodiment of the present invention, technical scheme is clearly and completely described, it is clear that institute
The embodiment of description is only part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention,
The every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, belongs to this hair
The scope of bright protection.
Embodiment 1
The evaporative crystallisation process of ox sulphur, its technological process is as shown in figure 1, comprise the following steps：
(1) after the taurine solution that concentration is 20% being heated into 80 DEG C, refined filtration processing is carried out by fine filter, is removed molten
Impurity in liquid, obtain taurine refined filtration liquid；
(2) taurine refined filtration liquid is delivered into evaporation concentrator, the feed rate for controlling taurine refined filtration liquid is 12m3/ h, steaming
Hair thickening temperature is 80 DEG C, vacuum is -50KPa in evaporation concentrator, is evaporated concentration, obtains concentrate；
(3) after concentrate concentration reaches 32%, deliver in crystallizing evaporator, the feed rate for controlling concentrate is 8m3/
H, evaporative crystallization temperature are 65 DEG C, are evaporated crystallization, when concentration reaches 40%, material reaches supersaturated shape in crystallizing evaporator
State, now stop charging, while it is 65 DEG C to control temperature, and 5000g granular sizes are added into crystallizing evaporator by crystal seed tank
For the taurine crystal seed of 80 mesh, and 30 minutes are incubated, during adding crystal seed, it is 65 DEG C control evaporative crystallization temperature, is evaporated
Vacuum is -98Kpa in crystallizer；Slowly enter concentrate afterwards until recovering to 8m3/ h, while temperature is controlled as 65 DEG C of progress
Evaporative crystallization；
(4) after the solid-to-liquid ratio of magma in crystallizing evaporator reaches 50%, magma continuous discharge is carried out, magma goes out
Stream amount is 6m3/ h, the magma of outflow are sent into maturator, and control maturator temperature is equal with the magma drop temperature temperature difference
Weighing apparatus, growing the grain 30 minutes；
(5) magma after growing the grain delivers to centrifuge and carries out continuous centrifugal separation, the taurine wet crystal after centrifugation
It is dried into dryer, you can obtain dry ox sulphur crystal, the smart mother liquor after centrifugation is directly entered material-compound tank
Carry out circular batching or return neutralization reaction kettle to carry out neutralisation treatment.
Embodiment 2
The evaporative crystallisation process of ox sulphur, its technological process is as shown in figure 1, comprise the following steps：
(1) after the taurine solution that concentration is 23% being heated into 60 DEG C, refined filtration processing is carried out by fine filter, is removed molten
Impurity in liquid, obtain taurine refined filtration liquid；
(2) taurine refined filtration liquid is delivered into evaporation concentrator, the feed rate for controlling taurine refined filtration liquid is 12m3/ h, steaming
Hair thickening temperature is 75 DEG C, vacuum is -60KPa in evaporation concentrator, is evaporated concentration, obtains concentrate；
(3) after concentrate concentration reaches 35%, deliver in crystallizing evaporator, the feed rate for controlling concentrate is 8m3/
H, evaporative crystallization temperature are 60 DEG C, are evaporated crystallization, when concentration reaches 38%, material reaches supersaturated shape in crystallizing evaporator
State, now stop charging, while it is 60 DEG C to control temperature, and 5000g granular sizes are added into crystallizing evaporator by crystal seed tank
For the taurine crystal seed of 90 mesh, and 50 minutes are incubated, during adding crystal seed, it is 60 DEG C control evaporative crystallization temperature, is evaporated
Vacuum is -80Kpa in crystallizer；Slowly enter concentrate afterwards until recovering to 8m3/ h, while temperature is controlled as 60 DEG C of progress
Evaporative crystallization；
(4) after the solid-to-liquid ratio of magma in crystallizing evaporator reaches 40%, magma continuous discharge is carried out, magma goes out
Stream amount is 5m3/ h, the magma of outflow are sent into maturator, and control maturator temperature is equal with the magma drop temperature temperature difference
Weighing apparatus, growing the grain 50 minutes；
(5) magma after growing the grain delivers to centrifuge and carries out continuous centrifugal separation, the taurine wet crystal after centrifugation
It is dried into dryer, you can obtain dry ox sulphur crystal, the smart mother liquor after centrifugation is directly entered material-compound tank
Carry out circular batching or return neutralization reaction kettle to carry out neutralisation treatment.
Embodiment 3
The evaporative crystallisation process of ox sulphur, its technological process is as shown in figure 1, comprise the following steps：
(1) after the taurine solution that concentration is 25% being heated into 70 DEG C, refined filtration processing is carried out by fine filter, is removed molten
Impurity in liquid, obtain taurine refined filtration liquid；
(2) taurine refined filtration liquid is delivered into evaporation concentrator, the feed rate for controlling taurine refined filtration liquid is 12m3/ h, steaming
Hair thickening temperature is 78 DEG C, vacuum is -55KPa in evaporation concentrator, is evaporated concentration, obtains concentrate；
(3) after concentrate concentration reaches 33%, deliver in crystallizing evaporator, the feed rate for controlling concentrate is 8m3/
H, evaporative crystallization temperature are 55 DEG C, are evaporated crystallization, when concentration reaches 38%, material reaches supersaturated shape in crystallizing evaporator
State, now stop charging, while it is 55 DEG C to control temperature, and 5000g granular sizes are added into crystallizing evaporator by crystal seed tank
For the taurine crystal seed of 100 mesh, and 60 minutes are incubated, during adding crystal seed, it is 55 DEG C control evaporative crystallization temperature, is evaporated
Vacuum is -90KPa in crystallizer；Slowly enter concentrate afterwards until recovering to 8m3/ h, while temperature is controlled as 55 DEG C of progress
Evaporative crystallization；
(4) after the solid-to-liquid ratio of magma in crystallizing evaporator reaches 45%, magma continuous discharge is carried out, magma goes out
Stream amount is 6m3/ h, the magma of outflow are sent into maturator, and control maturator temperature is equal with the magma drop temperature temperature difference
Weighing apparatus, growing the grain 60 minutes；
(5) magma after growing the grain delivers to centrifuge and carries out continuous centrifugal separation, the taurine wet crystal after centrifugation
It is dried into dryer, you can obtain dry ox sulphur crystal, the smart mother liquor after centrifugation is directly entered material-compound tank
Carry out circular batching or return neutralization reaction kettle to carry out neutralisation treatment.
Embodiment 4
The evaporative crystallisation process of ox sulphur, its technological process is as shown in figure 1, comprise the following steps：
(1) after the taurine solution that concentration is 22% being heated into 65 DEG C, refined filtration processing is carried out by fine filter, is removed molten
Impurity in liquid, obtain taurine refined filtration liquid；
(2) taurine refined filtration liquid is delivered into evaporation concentrator, the feed rate for controlling taurine refined filtration liquid is 12m3/ h, steaming
Hair thickening temperature is 80 DEG C, vacuum is -69KPa in evaporation concentrator, is evaporated concentration, obtains concentrate；
(3) after concentrate concentration reaches 34%, deliver in crystallizing evaporator, the feed rate for controlling concentrate is 8m3/
H, evaporative crystallization temperature are 65 DEG C, are evaporated crystallization, when concentration reaches 39%, material reaches supersaturated shape in crystallizing evaporator
State, now stop charging, while it is 65 DEG C to control temperature, and 5000g granular sizes are added into crystallizing evaporator by crystal seed tank
For the taurine crystal seed of 100 mesh, and 40 minutes are incubated, during adding crystal seed, it is 65 DEG C control evaporative crystallization temperature, is evaporated
Vacuum is -70KPa in crystallizer；Slowly enter concentrate afterwards until recovering to 8m3/ h, while temperature is controlled as 65 DEG C of progress
Evaporative crystallization；
(4) after the solid-to-liquid ratio of magma in crystallizing evaporator reaches 50%, magma continuous discharge is carried out, magma goes out
Stream amount is 5m3/ h, the magma of outflow are sent into maturator, and control maturator temperature is equal with the magma drop temperature temperature difference
Weighing apparatus, growing the grain 60 minutes；
(5) magma after growing the grain delivers to centrifuge and carries out continuous centrifugal separation, the taurine wet crystal after centrifugation
It is dried into dryer, you can obtain dry ox sulphur crystal, the smart mother liquor after centrifugation is directly entered material-compound tank
Carry out circular batching or return neutralization reaction kettle to carry out neutralisation treatment.
It should be noted that the evaporative crystallisation process of the present invention can also use single-action, Multi-effect evaporation crystallizer, DTB knots
The continuous evaporative crystallization equipment such as brilliant device or FC crystallizer.
Claims (4)
- A kind of 1. evaporative crystallisation process of ox sulphur, it is characterised in that：Comprise the following steps：(1) after the taurine solution that concentration is 20~25% being heated into 60~80 DEG C, refined filtration processing is carried out by fine filter, is removed Impurity in solution is removed, obtains taurine refined filtration liquid；(2) taurine refined filtration liquid is delivered into evaporation concentrator, the feed rate for controlling taurine refined filtration liquid is 12m3/ h, evaporation are dense Contracting temperature is 75~80 DEG C, vacuum is -50~-69KPa in evaporation concentrator, is evaporated concentration, obtains concentrate；(3) after concentrate concentration reaches 32%~35%, deliver in crystallizing evaporator, the feed rate for controlling concentrate is 8m3/ h, evaporative crystallization temperature are 55~65 DEG C, are evaporated crystallization, when concentration reaches 38%~40%, thing in crystallizing evaporator Material reaches hypersaturated state, now stops charging, while it is 55~65 DEG C to control temperature, by crystal seed tank into crystallizing evaporator 5000g taurine crystal seeds are added, and are incubated 30~60 minutes, slowly enter concentrate afterwards until recovering to 8m3/ h, is controlled simultaneously Temperature is 55~65 DEG C and is evaporated crystallization；(4) after the solid-to-liquid ratio of magma in crystallizing evaporator reaches 40~50%, magma continuous discharge is carried out, magma goes out Stream amount is 5~6m3/ h, the magma of outflow are sent into maturator, control maturator temperature and the magma drop temperature temperature difference Balance each other, growing the grain 30~60 minutes；(5) magma after growing the grain delivers to centrifuge and carries out continuous centrifugal separation, and the taurine wet crystal after centrifugation enters Dryer is dried, you can obtains dry ox sulphur crystal.
- 2. the evaporative crystallisation process of ox sulphur according to claim 1, it is characterised in that：Step (3) is in addition crystal seed During, it is 55~65 DEG C to control evaporative crystallization temperature, and vacuum is -70~-98KPa in crystallizing evaporator.
- 3. the evaporative crystallisation process of ox sulphur according to claim 1, it is characterised in that：After step (5) centrifuges Smart mother liquor is directly entered material-compound tank and carries out circular batching or return neutralization reaction kettle progress neutralisation treatment.
- 4. the evaporative crystallisation process of ox sulphur according to claim 1 or 2, it is characterised in that：Ox sulphur described in step (3) The granular size of sulphur crystal seed is 80~100 mesh.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710576241.4A CN107353235A (en) | 2017-07-14 | 2017-07-14 | A kind of evaporative crystallisation process of ox sulphur |
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| CN201710576241.4A CN107353235A (en) | 2017-07-14 | 2017-07-14 | A kind of evaporative crystallisation process of ox sulphur |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109574886A (en) * | 2018-11-19 | 2019-04-05 | 万华化学集团股份有限公司 | The taurine crystal and preparation method thereof that a kind of heap density, mobility are improved and do not coalesced |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104725284A (en) * | 2015-03-06 | 2015-06-24 | 集美大学 | Novel preparation method for natural taurine |
| CN105289025A (en) * | 2015-11-20 | 2016-02-03 | 潜江永安药业股份有限公司 | Double-effect concentration technology of taurine solution |
-
2017
- 2017-07-14 CN CN201710576241.4A patent/CN107353235A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104725284A (en) * | 2015-03-06 | 2015-06-24 | 集美大学 | Novel preparation method for natural taurine |
| CN105289025A (en) * | 2015-11-20 | 2016-02-03 | 潜江永安药业股份有限公司 | Double-effect concentration technology of taurine solution |
Non-Patent Citations (1)
| Title |
|---|
| 陆剑平等: "牛磺酸精结晶方法的研究", 《天津化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109574886A (en) * | 2018-11-19 | 2019-04-05 | 万华化学集团股份有限公司 | The taurine crystal and preparation method thereof that a kind of heap density, mobility are improved and do not coalesced |
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Application publication date: 20171117 |