CN110152340A - One kind dividing salt evaporative crystallization and purification process - Google Patents

One kind dividing salt evaporative crystallization and purification process Download PDF

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Publication number
CN110152340A
CN110152340A CN201810256858.2A CN201810256858A CN110152340A CN 110152340 A CN110152340 A CN 110152340A CN 201810256858 A CN201810256858 A CN 201810256858A CN 110152340 A CN110152340 A CN 110152340A
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CN
China
Prior art keywords
salt
purification process
sodium chloride
evaporative crystallization
purity
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201810256858.2A
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Chinese (zh)
Inventor
郭超
艾山·玉素莆
祖拜代·图尔荪麦麦提
杨泰山
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XINJIANG ENVIRONMENTAL ENGINEERING TECHNOLOGY Co Ltd
Original Assignee
XINJIANG ENVIRONMENTAL ENGINEERING TECHNOLOGY Co Ltd
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Publication date
Application filed by XINJIANG ENVIRONMENTAL ENGINEERING TECHNOLOGY Co Ltd filed Critical XINJIANG ENVIRONMENTAL ENGINEERING TECHNOLOGY Co Ltd
Priority to CN201810256858.2A priority Critical patent/CN110152340A/en
Publication of CN110152340A publication Critical patent/CN110152340A/en
Pending legal-status Critical Current

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0004Crystallisation cooling by heat exchange
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0018Evaporation of components of the mixture to be separated
    • B01D9/0031Evaporation of components of the mixture to be separated by heating
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D3/00Halides of sodium, potassium or alkali metals in general
    • C01D3/04Chlorides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D3/00Halides of sodium, potassium or alkali metals in general
    • C01D3/22Preparation in the form of granules, pieces, or other shaped products
    • C01D3/24Influencing the crystallisation process
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D5/00Sulfates or sulfites of sodium, potassium or alkali metals in general
    • C01D5/16Purification
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D2009/0086Processes or apparatus therefor

Abstract

The invention discloses one kind to divide salt evaporative crystallization and purification process, including flush distillation, freezing and crystallizing, four evaporation purification, double evaporation-cooling steps, the invention realizes printing and dyeing high-salt wastewater sodium sulphate and sodium chloride divides salt, and it ensure that the purity of sodium sulphate and sodium chloride, the salinity of sodium sulphate purity >=99%, sodium chloride purity >=98%, output can be back to use in industrial production, it is finally discharged without waste water and solid waste, realizes real zero-emission.

Description

One kind dividing salt evaporative crystallization and purification process
Technical field
The present invention relates to techniques of Dyeing Wastewater Treatment field, especially one kind divides salt evaporative crystallization and purification process.
Background technique
In recent years, the popularization with country to zero-discharge technology, zero-discharge technology have application to various highly difficult waste water Dyeing waste water in processing, especially in textile industry.
Dyeing waste water salt content is high, and direct emission is easy to bring ecological problem.It is largely helped used in printing and dyeing production process Agent, such as caustic soda, anhydrous sodium sulphate, soda ash, sodium chloride and can improve containing salt dyestuff salt content in waste water.High-salt wastewater such as without Desalination, direct emission will cause larger harm to the water quality of receiving water body, or even cause Secondary Saline.
It can only all accomplish the zero-emission of water for most of zero-discharge technologies for the treatment of of dyeing wastewater at present, in treatment process The salinity of generation is because of its broad categories and contains heavy metal substance, can only do dangerous waste processing, and saline pollution problem still remains, and It is not carried out real zero-emission.Therefore it how by the salt progress separating-purifying in high-salt wastewater in processing, is allowed to recycle, It realizes real zero-emission, is the key that high-salinity wastewater zero-emission technology.
Summary of the invention
Technical problems based on background technology, the present invention propose that one kind divides salt evaporative crystallization and purification process, for High saliferous printing and dyeing high-salt wastewater sodium sulphate and sodium chloride divide the technique of salt and purification, finally realize the zero-emission of high saliferous dyeing waste water It puts.
One kind dividing salt evaporative crystallization and purification process, and method and step is as follows:
S1: flush distillation: by the salt content of high-salt wastewater by (0.8-1.2) × 105Mg/L be concentrated into (2.8-3.2) × 105mg/L;
S2: freezing and crystallizing: the concentration waste water that S1 is obtained is delivered to freezing and crystallizing device, Na is precipitated2SO4·10H2O is brilliant Body, realization sodium sulphate and sodium chloride divide salt;
S3: evaporation purification: the Na that S2 is obtained2SO4·10H2O is evaporated purification, final 99% or more the purity of output Sodium sulfate salt;
S4: double evaporation-cooling: being evaporated crystallization for the mother liquor that S2 is obtained again, 98% or more sodium chloride salt of output purity, The mother liquor of double evaporation-cooling returns to flush distillation circular treatment.
Preferably, the temperature that flush distillation is concentrated in the S1 is 50-100 DEG C.
Preferably, the temperature of freezing and crystallizing is 0 DEG C in the S2.
Preferably, the temperature that double evaporation-cooling crystallizes in the S4 is 80-100 DEG C.
Salt evaporative crystallization and purification process is divided to be applied to the sulfuric acid in separation printing and dyeing high-salt wastewater the present invention also provides a kind of Sodium and sodium chloride.
It is in the present invention the utility model has the advantages that
The present invention proposes that one kind divides salt evaporative crystallization and purification process, the invention realize printing and dyeing high-salt wastewater sodium sulphate and Sodium chloride divides salt, and ensure that the purity of sodium sulphate and sodium chloride, sodium sulphate purity >=99%, sodium chloride purity >=98%, The salinity of output can be back to use in industrial production, be finally discharged without waste water and solid waste, realized real zero-emission.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with reality of the invention It applies example to be used to explain the present invention together, not be construed as limiting the invention.In the accompanying drawings:
Fig. 1 is a kind of flow chart for dividing salt evaporative crystallization and purification process proposed by the present invention.
Specific embodiment
Combined with specific embodiments below the present invention is made further to explain.
Embodiment 1
S1: flush distillation: by the salt content of high-salt wastewater by 0.8 × 105Mg/L is concentrated into 3.2 × 105Mg/L, it is primary to steam The temperature of hair concentration is 50 DEG C;
S2: freezing and crystallizing: the concentration waste water that S1 is obtained is delivered to freezing and crystallizing device, Na is precipitated2SO4·10H2O is brilliant Body, realization sodium sulphate and sodium chloride divide salt, and the temperature of freezing and crystallizing is 0 DEG C;
S3: evaporation purification: the Na that S2 is obtained2SO4·10H2O is evaporated purification, the sulphur of the final purity 99.3% of output Acid sodium-salt;
S4: double evaporation-cooling: being evaporated crystallization for the mother liquor that S2 is obtained again, the sodium chloride salt of output purity 98.2%, The temperature of double evaporation-cooling crystallization is 80 DEG C, and the mother liquor reflux of evaporation residue is intake to flush distillation, circular treatment.
Embodiment 2
S1: flush distillation: by the salt content of high-salt wastewater by 1.2 × 105Mg/L is concentrated into 2.8 × 105Mg/L, it is primary to steam The temperature of hair concentration is 100 DEG C;
S2: freezing and crystallizing: the concentration waste water that S1 is obtained is delivered to freezing and crystallizing device, Na is precipitated2SO4·10H2O is brilliant Body, realization sodium sulphate and sodium chloride divide salt, and the temperature of freezing and crystallizing is 0 DEG C;
S3: evaporation purification: the Na that S2 is obtained2SO4·10H2O is evaporated purification, the sulphur of the final purity 99.5% of output Acid sodium-salt;
S4: double evaporation-cooling: being evaporated crystallization for the mother liquor that S2 is obtained again, the sodium chloride salt of output purity 98.6%, The temperature of double evaporation-cooling crystallization is 100 DEG C, and the mother liquor reflux of evaporation residue is intake to flush distillation, circular treatment.
Embodiment 3
S1: flush distillation: by the salt content of high-salt wastewater by 1.0 × 105Mg/L is concentrated into 3.0 × 105Mg/L, it is primary to steam The temperature of hair concentration is 80 DEG C;
S2: freezing and crystallizing: the concentration waste water that S1 is obtained is delivered to freezing and crystallizing device, Na is precipitated2SO4·10H2O is brilliant Body, realization sodium sulphate and sodium chloride divide salt, and the temperature of freezing and crystallizing is 0 DEG C;
S3: evaporation purification: the Na that S2 is obtained2SO4·10H2O is evaporated purification, the sulphur of the final purity 99.3% of output Acid sodium-salt;
S4: double evaporation-cooling: being evaporated crystallization for the mother liquor that S2 is obtained again, the sodium chloride salt of output purity 98.5%, The temperature of double evaporation-cooling crystallization is 90 DEG C, and the mother liquor reflux of evaporation residue is intake to flush distillation, circular treatment.
Detection test
1) 100g sodium sulphate made from Example 3 produces salt and carries out content detection, the results are shown in Table 1.
1 sodium sulphate of table produces salt component
Produce salt total amount Sodium sulphate Sodium chloride Potassium chloride Potassium sulfate Other substances Sodium sulphate purity
100g 99.58g 0.37g 0.025g 0.012g 0.013g 99.58%
2) 100g sodium chloride made from Example 3 produces salt and carries out content detection, the results are shown in Table 2.
2 sodium chloride of table produces salt component
Produce salt total amount Sodium sulphate Sodium chloride Potassium chloride Potassium sulfate Other substances Sodium sulphate purity
100g 1.11g 98.77g 0.05g 0.025g 0.045g 98.77%
3) double evaporation-cooling mother liquor water quality is shown in Table 3 in embodiment 3.
The component of 3 double evaporation-cooling mother liquor of table
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto, Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.

Claims (5)

1. one kind divides salt evaporative crystallization and purification process, which is characterized in that method and step is as follows:
S1: flush distillation: by the salt content of high-salt wastewater by (0.8-1.2) × 105Mg/L is concentrated into (2.8-3.2) × 105mg/ L;
S2: freezing and crystallizing: the concentration waste water that S1 is obtained is delivered to freezing and crystallizing device, Na is precipitated2SO4·10H2O crystal, it is real Existing sodium sulphate and sodium chloride divide salt;
S3: evaporation purification: the Na that S2 is obtained2SO4·10H2O is evaporated purification, the sulfuric acid of final 99% or more the purity of output Sodium salt;
S4: double evaporation-cooling: the mother liquor that S2 is obtained is evaporated crystallization again, 98% or more sodium chloride salt of output purity is secondary The mother liquor of evaporation returns to flush distillation circular treatment.
2. one kind according to claim 1 divides salt evaporative crystallization and purification process, which is characterized in that once steamed in the S1 The temperature of hair concentration is 50-100 DEG C.
3. one kind according to claim 1 divides salt evaporative crystallization and purification process, which is characterized in that freeze knot in the S2 Brilliant temperature is 0 DEG C.
4. one kind according to claim 1 divides salt evaporative crystallization and purification process, which is characterized in that secondary steaming in the S4 The temperature of hair crystallization is 80-100 DEG C.
5. the described in any item one kind of claim 1-4 divide salt evaporative crystallization and purification process to be applied to separation printing and dyeing high-salt wastewater In sodium sulphate and sodium chloride.
CN201810256858.2A 2018-03-27 2018-03-27 One kind dividing salt evaporative crystallization and purification process Pending CN110152340A (en)

Priority Applications (1)

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Publications (1)

Publication Number Publication Date
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111704294A (en) * 2020-06-04 2020-09-25 徐翔 General recycling process for fine chemical wastewater
CN112707417A (en) * 2021-01-14 2021-04-27 江苏赛德力制药机械制造有限公司 Sodium sulfate and sodium chloride salt separation method

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102452672A (en) * 2010-11-01 2012-05-16 中国石油化工股份有限公司 Method for recycling sodium sulfate from waste alkali liquor of ethylene unit
CN105036222A (en) * 2015-08-19 2015-11-11 石家庄工大化工设备有限公司 High-salinity wastewater recovery treatment method
CN106007133A (en) * 2016-05-27 2016-10-12 苏州乔发环保科技股份有限公司 Desulfurization wastewater concentration, evaporation, crystallization and salt separation process
CN106315991A (en) * 2016-10-11 2017-01-11 内蒙古中煤远兴能源化工有限公司 Industrial wastewater salt separation technology and industrialized application thereof
CN107619144A (en) * 2017-10-20 2018-01-23 侯新春 A kind of high slat-containing wastewater divides salt process for reclaiming and system

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102452672A (en) * 2010-11-01 2012-05-16 中国石油化工股份有限公司 Method for recycling sodium sulfate from waste alkali liquor of ethylene unit
CN105036222A (en) * 2015-08-19 2015-11-11 石家庄工大化工设备有限公司 High-salinity wastewater recovery treatment method
CN106007133A (en) * 2016-05-27 2016-10-12 苏州乔发环保科技股份有限公司 Desulfurization wastewater concentration, evaporation, crystallization and salt separation process
CN106315991A (en) * 2016-10-11 2017-01-11 内蒙古中煤远兴能源化工有限公司 Industrial wastewater salt separation technology and industrialized application thereof
CN107619144A (en) * 2017-10-20 2018-01-23 侯新春 A kind of high slat-containing wastewater divides salt process for reclaiming and system

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111704294A (en) * 2020-06-04 2020-09-25 徐翔 General recycling process for fine chemical wastewater
CN112707417A (en) * 2021-01-14 2021-04-27 江苏赛德力制药机械制造有限公司 Sodium sulfate and sodium chloride salt separation method

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