CN100375714C - Process for preparing anhydrous mirabilite by freezing method - Google Patents
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- CN100375714C CN100375714C CNB2006100134586A CN200610013458A CN100375714C CN 100375714 C CN100375714 C CN 100375714C CN B2006100134586 A CNB2006100134586 A CN B2006100134586A CN 200610013458 A CN200610013458 A CN 200610013458A CN 100375714 C CN100375714 C CN 100375714C
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Abstract
The present invention discloses a novel process for producing anhydrous sulfate by a refrigeration method, which comprises the following steps: the cooling medium primary cooling of solution containing sulfate is carried out by mother liquid through a precooler; feed liquid coming out of the precooler is transferred to a precooling crystallizer; the feed liquid coming out of the precooling crystallizer is sent to a refrigeration crystallizer, the feed liquid is refrigerated to -5 to -7 DEG C for second phase refrigeration for sulfate separation; the feed liquid refrigerated by the refrigeration crystallizer is sent to a depressor for solid-liquid separation; the material feeding of sodium sulfate slurry discharged from the bottom of the depressor is carried out by a dehydrator through a screw pump; the sodium sulfate after the dehydration enters a sulfate dissolution tank to be mixed with the feed liquid discharged by evaporation or anhydrous sulfate slurry dripped liquid and heated by end effect secondary steam to ebable the sodium sulfate to be autolyzed. The sulfate dissolution processes of the method adopt a hot material and the sodium sulfate to dissolve the sulfate in a mixed mode and simultaneously use low quality secondary steam heat energy to heat the feed liquid. Compared with the original total dissolution evaporation method, the method is more reasonable and more energy-saving and ensures the quality of products.
Description
Technical field
The present invention relates to a kind of anhydrous nitre production technique, the invention particularly relates to a kind of anhydrous mirabilite by freezing method production technique.
Background technology
Present anhydrous nitre production technique has only the freezing system nitre of ammonia system, and does not adopt chilled brine to do the utilisation technology of refrigerant.As everyone knows, produce anhydrous nitre by saltcake and mainly contain complete molten method of evaporation and salting-out process.The former quality product is secure, but power consumption is high; Though the latter is energy-conservation, change nitre with salt, final product quality instability.
Summary of the invention
The object of the present invention is to provide a kind of anhydrous mirabilite by freezing method production technique, adopt this technology both to guarantee the quality of product, reached purpose of energy saving again.
A kind of process for preparing anhydrous mirabilite by freezing method of the present invention, it may further comprise the steps:
(a) will contain nitre solution, and do refrigerant by pre-cooler by cold mother liquor and tentatively be cooled to 10-20 ℃;
(b) will change pre-cooling crystallizer from the feed liquid that pre-cooler comes out over to, the refrigerant of pre-cooling crystallizer adopt temperature for-4 ℃-5 ℃ cold mother liquor to feed liquid carry out one section freezing;
(c) will send into the freezing and crystallizing device from the feed liquid that pre-cooling crystallizer comes out feed liquid is refrigerated to-5--7 ℃ carries out two sections freezing nitre of analysing; The refrigerant of freezing and crystallizing device is by the freezing calcium chloride brine of the temperature that provides of refrigeration operation for-8--12 ℃;
(d) feed liquid after the freezing and crystallizing device is freezing is sent into the settling vessel solid-liquid separation;
(e) the saltcake slurry of being discharged by the settling vessel bottom is given the water extracter feeding through spiral pump;
(f) entering of the saltcake nitre jar after the dehydration, getting rid of back liquid with feed liquid of evaporating discharge or anhydrous nitre slurry mixes, and heat with end effect secondary steam, temperature is changed nitre at 40 ℃-50 ℃ in the controlling tank, make the saltcake self-dissolving, the anhydrous nitre slurry of after this discharging is made wet anhydrous nitre through dehydration, and wet anhydrous nitre obtains anhydrous nitre product after drying, the feed liquid that described evaporation is discharged is the anhydrous nitre solution of contains sodium sulfate xln, and it is metabisulfite solution that described anhydrous nitre slurry gets rid of back liquid;
The mother liquor that the refrigerant of described (a) and (b) step adopts is the cold mother liquor of settling vessel overflow in (d) step, and described cold mother liquor successively is used as the refrigerant of pre-cooling crystallizer, pre-cooler in two steps.
Present method saltcake slurry adopts the spiral pump feed, is more convenient for operating than former steel basin and impeller pump feed.Changing the nitre operation, adopted hot material and saltcake hybridization nitre, heat to feed liquid with low-grade secondary steam heat energy simultaneously, more reasonable, more energy-conservation than former complete molten method of evaporation.Present technique is to make the abundant self-dissolving of saltcake, and only evaporates the residue mother liquor after the self-dissolving, has both guaranteed the quality of product, has reached purpose of energy saving again.And make the refrigerated heat transfer temperature difference more reasonable, prolonged the brush jar cycle, an existing brush jar cycle is 3-6 month.
Description of drawings
Fig. 1 is the schema of a kind of anhydrous mirabilite by freezing method production technique of the present invention;
Fig. 2 is the structural representation of the change nitre jar of the inventive method employing.
Embodiment
Below in conjunction with the drawings and specific embodiments the present invention is done to describe in detail.
The inventive method is to contain nitre solution (salt made from earth containing a comparatively high percentage of sodium chloride water) as shown in Figure 1, does refrigerant by pre-cooler by the cold mother liquor (liquid salt) of lesser temps and tentatively is cooled to 10-20 ℃.Again feed liquid is changed over to pre-cooling crystallizer.The refrigerant of pre-cooling crystallizer adopts temperature to be-4 ℃--5 ℃ of cold mother liquors (liquid salt) to feed liquid carry out one section freezing.After enter the freezing and crystallizing device and carry out two sections freezing nitre of analysing.The refrigerant of freezing and crystallizing device is to be-8--12 ℃ chilled brine by the temperature that the refrigeration operation provides.Feed liquid is refrigerated to-5--7 ℃, chilled brine is discharged refrigeration system, and described chilled brine is a calcium chloride brine.Feed liquid after freezing enters the settling vessel solid-liquid separation.The cold mother liquor of settling vessel overflow successively is used as the refrigerant of pre-cooling crystallizer, pre-cooler in two steps.Discharge system as liquid salt then.By the saltcake slurry that discharge the settling vessel bottom, give the water extracter feeding through spiral pump.Get rid of back liquid because of containing the saltcake crystallite, pump to freezing and crystallizing device can be used as crystal seed and continues freezing.Entering of saltcake nitre jar after the dehydration gets rid of back liquid with feed liquid of evaporating discharge or anhydrous nitre slurry and mixes, and heats with end effect secondary steam, and controlled temperature 40-50 ℃ of change nitre makes the saltcake self-dissolving.The anhydrous nitre slurry of after this discharging is made wet anhydrous nitre through dehydration.Anhydrous nitre gets rid of back liquid and enters vapo(u)rization system, or later changes nitre.Certainly, if get rid of back liquid being used to nitre, this feed liquid direct evaporation then, it is higher that the feed liquid solid-to-liquid ratio is finished in evaporation, can dewater and isolate wet anhydrous nitre.The feed liquid that described evaporation is discharged is the anhydrous nitre solution of contains sodium sulfate xln, and it is metabisulfite solution that described anhydrous nitre slurry gets rid of back liquid.
The change nitre jar that adopts in the inventive method can be replaced by the change nitre equipment of other type of buying on the ordinary city field, but preferably adopt equipment disclosed by the invention, can play better heat exchange and energy-conserving action like this, equipment of the present invention as shown in drawings, a kind ofization nitre jar, it comprises tank body 9, the lower tube box 2 that links to each other with described tank body 9 bottoms, be provided with the center in described tank body central authorities and take over 8, the bottom was provided with shell and tube heat exchanger 7 around described center was taken over, the steam that described tank wall is provided with described shell and tube heat exchanger advances 3, outlet 4, the balance mouth of pipe 5, condensation-water drain 6, described tank body roof are provided with ten water nitre inlet pipes 10.Because last process evaporating pot tank body need keep vacuum when operation, nitre slurry inlet pipe 11 body bottoms are arranged in the described pipe core, can play the fluid-tight effect.Its outer wall of part that described nitre slurry inlet pipe is preferably disposed in the adapter of described center leans against on the inwall of taking at described center, like this can be so that circulating effect is better.Described lower tube box bottom is connected with propeller pump 1, and the blade of described propeller pump is arranged on the pipe inner bottom part that described center is taken over.Have nitre slurries outlet 12 on the described lower tube box bottom shell sidewall.Described tank body upper portion side wall is provided with manhole 13.Described center is taken over the top and is satisfied liquid apart from the distance of tank body roof and can keep circulation get final product, and the caliber that described center is taken over satisfies feed liquid and circulates and get final product.
With mass concentration is that the nitre solution that contains of 70g/1 is done refrigerant by pre-cooler by cold mother liquor and tentatively is cooled to 10 ℃.Again feed liquid is changed over to pre-cooling crystallizer.The refrigerant of pre-cooling crystallizer adopt temperature for-4 ℃ of cold mother liquors to feed liquid carry out one section freezing.After enter the freezing and crystallizing device and carry out two sections freezing nitre of analysing.The refrigerant of freezing and crystallizing device is feed liquid to be refrigerated to-6 ℃ by the temperature that the refrigeration operation provides for-10 ℃ of freezing calcium chloride brine, and calcium chloride brine is discharged refrigeration system.Feed liquid after freezing enters the settling vessel solid-liquid separation.The cold mother liquor of settling vessel overflow successively is used as the refrigerant of pre-cooling crystallizer, pre-cooler in two steps.Discharge system as liquid salt then.By the saltcake slurry that discharge the settling vessel bottom, give the water extracter feeding through spiral pump.Get rid of back liquid because of containing the saltcake crystallite, pump to freezing and crystallizing device can be used as crystal seed and continues freezing.Entering of saltcake nitre jar after the dehydration mixes with the feed liquid that evaporation is discharged, and heats with end effect secondary steam, and controlled temperature is changed nitre for 45 ℃, makes the saltcake self-dissolving.The anhydrous nitre slurry of after this discharging is made wet anhydrous nitre through dehydration, and it is 99.3% sodium sulfate finished product that wet anhydrous nitre obtains the quality percent purity after drying.
With mass concentration is that the nitre solution that contains of 65g/1 is done refrigerant by pre-cooler by cold mother liquor and tentatively is cooled to 15 ℃.Again feed liquid is changed over to pre-cooling crystallizer.The refrigerant of pre-cooling crystallizer adopt temperature for-5 ℃ of cold mother liquors to feed liquid carry out one section freezing.After enter the freezing and crystallizing device and carry out two sections freezing nitre of analysing.The refrigerant of freezing and crystallizing device is feed liquid to be refrigerated to-5 ℃ by the temperature that provides of refrigeration operation for-8 ℃ freezing calcium chloride brine, and freezing calcium chloride brine is discharged refrigeration system.Feed liquid after freezing enters the settling vessel solid-liquid separation.The cold mother liquor of settling vessel overflow successively is used as the refrigerant of pre-cooling crystallizer, pre-cooler in two steps.Discharge system as liquid salt then.By the saltcake slurry that discharge the settling vessel bottom, give the water extracter feeding through spiral pump.Get rid of back liquid because of containing the saltcake crystallite, pump to freezing and crystallizing device can be used as crystal seed and continues freezing.The ten water nitre inlet pipes that saltcake after the dehydration enters of the present inventionization nitre jar get rid of back liquid with the anhydrous nitre slurry that enters nitre slurry inlet pipe to be mixed, and end effect secondary steam feeds the heating of shell and tube heat exchanger steam inlet, and temperature makes the saltcake self-dissolving at 50 ℃ of change nitre in the controlling tank.The anhydrous nitre slurry of after this discharging is made wet anhydrous nitre through dehydration.It is 99.0% sodium sulfate finished product that wet anhydrous nitre obtains the quality percent purity after drying.
With mass concentration is that the nitre solution that contains of 65g/l is done refrigerant by pre-cooler by cold mother liquor and tentatively is cooled to 20 ℃.Again feed liquid is changed over to pre-cooling crystallizer.The refrigerant of pre-cooling crystallizer adopt temperature for-5 ℃ of cold mother liquors to feed liquid carry out one section freezing.After enter the freezing and crystallizing device and carry out two sections freezing nitre of analysing.The refrigerant of freezing and crystallizing device is feed liquid to be refrigerated to-7 ℃ by the temperature that the refrigeration operation provides-12 ℃ of freezing calcium chloride brine, and calcium chloride brine is discharged refrigeration system.Feed liquid after freezing enters the settling vessel solid-liquid separation.The cold mother liquor of settling vessel overflow successively is used as the refrigerant of pre-cooling crystallizer, pre-cooler in two steps.Discharge system as liquid salt then.By the saltcake slurry that discharge the settling vessel bottom, give the water extracter feeding through spiral pump.Get rid of back liquid because of containing the saltcake crystallite, pump to freezing and crystallizing device can be used as crystal seed and continues freezing.Entering of saltcake nitre jar after the dehydration mixes with the feed liquid that evaporation is discharged, and heats with end effect secondary steam, and controlled temperature is changed nitre at 40 ℃, makes the saltcake self-dissolving.The anhydrous nitre slurry of after this discharging is made wet anhydrous nitre through dehydration.It is 98.0% sodium sulfate finished product that wet anhydrous nitre obtains the quality percent purity after drying.
Claims (4)
1. anhydrous mirabilite by freezing method production technique is characterized in that it may further comprise the steps:
(a) will contain nitre solution, and do refrigerant by pre-cooler by cold mother liquor and tentatively be cooled to 10-20 ℃;
(b) will change pre-cooling crystallizer from the feed liquid that pre-cooler comes out over to, the refrigerant of pre-cooling crystallizer adopt temperature for-4 ℃-5 ℃ cold mother liquor to feed liquid carry out one section freezing;
(c) will send into the freezing and crystallizing device from the feed liquid that pre-cooling crystallizer comes out feed liquid is refrigerated to-5--7 ℃ carries out two sections freezing nitre of analysing; The refrigerant of freezing and crystallizing device is by the freezing calcium chloride brine of the temperature that provides of refrigeration operation for-8--12 ℃;
(d) feed liquid after the freezing and crystallizing device is freezing is sent into the settling vessel solid-liquid separation;
(e) the saltcake slurry of being discharged by the settling vessel bottom is given the water extracter feeding through spiral pump;
(f) entering of the saltcake nitre jar after the dehydration, getting rid of back liquid with feed liquid of evaporating discharge or anhydrous nitre slurry mixes, and heat with end effect secondary steam, temperature is changed nitre at 40 ℃-50 ℃ in the controlling tank, make the saltcake self-dissolving, the anhydrous nitre slurry of after this discharging is made wet anhydrous nitre through dehydration, and wet anhydrous nitre obtains anhydrous nitre product after drying, the feed liquid that described evaporation is discharged is the anhydrous nitre solution that contains the sulfate crystal body, and it is metabisulfite solution that described anhydrous nitre slurry gets rid of back liquid;
The mother liquor that the refrigerant of described (a) and (b) step adopts is the cold mother liquor of settling vessel overflow in (d) step, and described cold mother liquor successively is used as the refrigerant of pre-cooling crystallizer, pre-cooler in two steps.
2. anhydrous mirabilite by freezing method production technique according to claim 1 is characterized in that: get rid of back liquid pump to freezing and crystallizing device in described (f) step and continue freezing as crystal seed.
3. anhydrous mirabilite by freezing method production technique according to claim 1, it is characterized in that: the change nitre jar in the described step (f), it comprises tank body, the lower tube box that links to each other with described tank base, being provided with the center in described tank body central authorities takes over, described center is provided with shell and tube heat exchanger around taking over the bottom, the steam that described tank wall is provided with described shell and tube heat exchanger advances, outlet, the balance mouth of pipe and the condensation mouth of a river, described tank body roof is respectively arranged with ten water nitre inlet pipes, its body bottom is arranged on the nitre slurry inlet pipe in the described pipe core, described lower tube box bottom is connected with propeller pump, the blade of described propeller pump is arranged on the pipe inner bottom part that described center is taken over, and has the outlet of nitre slurries on the described lower tube box bottom shell sidewall.
4. according to claim 3ization nitre jar, it is characterized in that: described tank body upper portion side wall is provided with manhole.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100134586A CN100375714C (en) | 2006-04-14 | 2006-04-14 | Process for preparing anhydrous mirabilite by freezing method |
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| CNB2006100134586A CN100375714C (en) | 2006-04-14 | 2006-04-14 | Process for preparing anhydrous mirabilite by freezing method |
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| CN100375714C true CN100375714C (en) | 2008-03-19 |
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| CN102092880B (en) * | 2010-12-01 | 2013-06-12 | 新疆天业（集团）有限公司 | Process for freezing and denitriding primary brine with membrane method in polyvinyl chloride production |
| CN102180487A (en) * | 2011-03-30 | 2011-09-14 | 湖南新澧化工有限公司 | Method for recycling saltpeter-production dead steam |
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| CN102320630A (en) * | 2011-09-05 | 2012-01-18 | 湖南衡阳新澧化工有限公司 | Production method of anhydrous sodium sulfate and production equipment thereof |
| CN102530998B (en) * | 2012-03-02 | 2013-12-04 | 化工部长沙设计研究院 | Bloedite mineralizing brine mixing clear liquid nitre freezing process |
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| CN104310437B (en) * | 2014-10-11 | 2016-04-13 | 中国轻工业长沙工程有限公司 | The anhydrous nitre technique of saltcake system |
| CN104310433B (en) * | 2014-10-11 | 2016-10-05 | 中国轻工业长沙工程有限公司 | High nitre brine freezing denitration continuous producing method |
| CN104528770A (en) * | 2014-12-23 | 2015-04-22 | 湘潭大学 | Mirabilite dehydration method based on gas-liquid direct heat exchange |
| CN106745079A (en) * | 2015-11-23 | 2017-05-31 | 湖南衡阳新澧化工有限公司 | A kind of production method of glauber salt |
| CN107617229A (en) * | 2016-07-13 | 2018-01-23 | 南风化工集团股份有限公司 | A kind of high efficiency energy saving refrigeration system of no refrigerating medium |
| CN109775727B (en) * | 2019-02-22 | 2021-05-11 | 江西赣锋锂业股份有限公司 | Continuous freezing crystallization process for mirabilite |
| CN112573544B (en) * | 2020-12-28 | 2022-12-27 | 江苏容汇通用锂业股份有限公司 | Method for separating sodium and potassium from lithium hydroxide mother liquor |
| CN115321725A (en) * | 2022-08-29 | 2022-11-11 | 徐州天嘉食用化工有限公司 | Disodium hydrogen phosphate recovery device for industrial wastewater treatment and recovery method thereof |
| CN117146483B (en) * | 2023-09-06 | 2024-03-26 | 内蒙古伊东集团东兴化工有限责任公司 | Heat exchange device and heat exchange method of denitration refrigerating unit by substituted membrane method |
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| CN1257834A (en) * | 1998-12-20 | 2000-06-28 | 内蒙古伊克昭化工研究设计院 | Process and equipment for preparing bittern mirabilite and separating anhydrous sodium sulfide |
| CN1608996A (en) * | 2004-10-09 | 2005-04-27 | 温润宪 | Method of separating sodium sulfate crystal from mirabilite mineral |
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2006
- 2006-04-14 CN CNB2006100134586A patent/CN100375714C/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1257834A (en) * | 1998-12-20 | 2000-06-28 | 内蒙古伊克昭化工研究设计院 | Process and equipment for preparing bittern mirabilite and separating anhydrous sodium sulfide |
| CN1608996A (en) * | 2004-10-09 | 2005-04-27 | 温润宪 | Method of separating sodium sulfate crystal from mirabilite mineral |
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Assignee: China National Technology Import & Export Corp. Assignor: China Salt Engineering Technology Research Institute Contract fulfillment period: 2008.8.3 to 2013.8.3 Contract record no.: 2009110000195 Denomination of invention: Process for preparing anhydrous mirabilite by freezing method Granted publication date: 20080319 License type: Exclusive license Record date: 20090911 |
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