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CN106757134A - A kind of production technology of anti-caking sodium chlorate - Google Patents

A kind of production technology of anti-caking sodium chlorate Download PDF

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Publication number
CN106757134A
CN106757134A CN201510831961.1A CN201510831961A CN106757134A CN 106757134 A CN106757134 A CN 106757134A CN 201510831961 A CN201510831961 A CN 201510831961A CN 106757134 A CN106757134 A CN 106757134A
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sodium chlorate
caking
solution
surfactant
production technology
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CN201510831961.1A
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张海波
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HUNAN HENGGUANG CHEMICAL CO Ltd
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HUNAN HENGGUANG CHEMICAL CO Ltd
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Abstract

A kind of production technology of anti-caking sodium chlorate, comprises the following steps:(1)The Crystallization Separation sodium chlorate from sodium chlorate electrolyte;(2)By step(1)The sodium chlorate for obtaining, saturation sodium chlorate solution is standby for preparation, takes above-mentioned saturation sodium chlorate solution 500ml, is placed in beaker, 2-5g surfactants are added, stirring makes surfactant be dissolved in above-mentioned saturation sodium chlorate solution, 500g sodium chlorate crystals are added, is stirred, stand ten minutes;(3)By step(2)Feed liquid vacuum filtration, will have been adsorbed surfactant sodium chlorate crystal be placed in 12-15 DEG C of thermostatic drying chamber dry;(4)Dried sodium chlorate is fitted into plastic sample bag, sealing.Preventing blocking effect of the present invention is good, and reagent dosage is few, and expense is low.

Description

A kind of production technology of anti-caking sodium chlorate
Technical field
The invention belongs to chemical technology field, a kind of production technology of anti-caking sodium chlorate is specifically referred to.
Background technology
During Applied In The Electrolytic Production of Sodium Chlorate, in order to complete to extract crystal sodium chlorate product in liquid from electrolysis, evaporation concentration method or freezing of saltouing can be used, after the crystal sodium chlorate of above two method production is placed one week, there is serious caking phenomenon, very big inconvenience is brought to user, the developing of overseas market is also have impact on.Therefore, carrying out the research work of sodium chlorate preventing blocking technology turns into the important topic of our factory technical staff.Sodium chlorate finished product belongs to inorganic salt crystal, and the selection of domestic and international inorganic salt crystal anti-caking additive substantially has two methods.One is to separate particle surface with some inert powders, prevents contact surface between particle excessive and produces bridging to act on.But if the method addition agent dose is very little, preventing blocking effect is poor;Addition agent dose is too big, and finished product purity is difficult to control within target level of product quality, i.e. impurity content exceeding index.Two is addition surfactant, and the hydrophobicity and other surfaces characteristic of inorganic salts plane of crystal are changed with surfactant.Surfactant additive amount is few in the method, will not change the original purity of inorganic salt crystal.
Inorganic salts caking mechanism, at present it is generally accepted that crystal bridge theory and capillary attraction are theoretical.The viewpoint of crystal bridge theory is the change with external condition due to itself, and the moisture included in crystal promotes plane of crystal to dissolve, and recrystallizes, so as to form crystal brige at crystal hole.Over time, these crystallizations are combined each other again, gradually form huge agglomerate.Capillary attraction theory thinks:Due to the presence of capillary attraction power between crystal, increase gaps between crystals saturated vapor pressure, promote crystal or plane of crystal to dissolve to form saturation or supersaturated drop, further recrystallization, is finally bonded to agglomerate.Surfactant prevents the inorganic salts caking mechanism from being:Surfactant molecule is adsorbed on the active site of plane of crystal, forms a kind of molecule " coating film ".This " coating film " thickness is nano level, and hydrophobic effect is good, is the main cause for preventing the sodium chlorate moisture absorption from luming.But, present conventional reagents carry out the effect of sodium chlorate anti-caking and bad.
Therefore, necessary a kind of production technology of anti-caking sodium chlorate of design.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of production technology of anti-caking sodium chlorate.
Present disclosure includes:
A kind of production technology of anti-caking sodium chlorate, comprises the following steps:
(1) the Crystallization Separation sodium chlorate from sodium chlorate electrolyte, sodium chlorate electrolyte is mixed to get density for 1.30~1.40g/cm with appropriate mother liquor3Mixed liquor, heating in vacuum simultaneously make mixed liquor in 35~45 DEG C boiling;Wherein, described mother liquor is that the crystallization of sodium chlorate electrolyte is separated out and separates remaining solution after sodium chlorate, the NaCl concentration≤130g/L in mother liquor;Mixed liquor density is 1.50~1.60g/cm3When, stop heating;Discharging, cooling, filtering, washing is dried, and obtains sodium chlorate;
(2) sodium chlorate for obtaining step (1), prepare saturation sodium chlorate solution standby, take above-mentioned saturation sodium chlorate solution 500ml, it is placed in beaker, adds 2-5g surfactants, stirring, surfactant is set to be dissolved in above-mentioned saturation sodium chlorate solution, 500g sodium chlorate crystals are added, is stirred, stand ten minutes;
(3) by the feed liquid vacuum filtration of step (2), the sodium chlorate crystal that will have been adsorbed surfactant is placed in drying in 12-15 DEG C of thermostatic drying chamber;
(4) dried sodium chlorate is fitted into plastic sample bag, sealing.
In the present invention, as a kind of perferred technical scheme, in step (1), described sodium chlorate electrolyte is the solution of refined brine gained after electrolysis.
In the present invention, as a kind of perferred technical scheme, in step (2), surfactant is using fatty glyceride and the mixture of fatty acid sorbitan.
In the present invention, as a kind of perferred technical scheme, the mass ratio of fatty glyceride and fatty acid sorbitan is (3-5):2.
In the present invention, as a kind of perferred technical scheme, in step (3), drying time is 2-5h.
The beneficial effects of the invention are as follows,
The addition manner of surfactant has various.Such as:Surfactant is participated in inorganic salts crystallization and inorganic salts is reached anti-caking purpose, crystalline mother solution is recycled in the method can influence other operation normal operatings.Inventor is soluble in water surfactant, and aqueous surfactant solution is added in inorganic salts finished product with spray mode, and drying, the uniformity that the method surfactant is distributed in inorganic salt product is poor, can also influence other operation normal operatings.By multi-party research and probe, the optimal experimental technique of inventor's design is that surfactant is dissolved in saturation sodium chlorate solution, crystal sodium chlorate is placed in again immersion ten minutes is stirred in above-mentioned saturated solution, filtering, resulting sodium chlorate crystal uniformly forms a kind of surfactant molecule " coating film ".This " coating film " hydrophobic effect is good, and to sodium chlorate anti-moisture absorption, anti-caking plays an important role, and this method does not change the original internal structure of sodium chlorate crystal.Above-mentioned filtrate is still the sodium chlorate saturated solution containing surfactant, is reclaimed and used, and surfactant is added operation and forms closed cycle, and surfactant does not flow into other operations of production of sodium chlorate, thus does not influence production.
Anti-caking chloric acid sodium sample after being processed by surfactant and the common chloric acid sodium sample without surfactant treatment reach country-level product standard.Through preliminary business accounting, one ton of anti-caking sodium chlorate of production need to increase by 20 yuan of anti-caking agent expense.The surface tension of the anti-caking sodium chlorate saturated solution processed through surfactant in the present invention is than common atmosphere acid sodium reduction by 24.7%, the reduction of surface tension, reduce the contact angle between solid-liquid, from capillary attraction caking theoretically, equivalent to the capillary attraction power reduced between material particles, the caking capacity of sour sodium crystal is grabbed so as to reduce.Its mechanism is probably:Atmosphere acid sodium product after surfactant treatment, (although there is " coating film " to generate after moisture absorption under storage requirement, but it is also impossible to the exchange for avoiding part moisture completely), moisture is between particle or when particle surface forms a certain degree of liquid film, adsorb surfactant molecule on crystal it is total some enter solution, so as to reduce the surface tension of solution, and the solid-liquid contact angle of liquid film is changed, be greatly reduced the capillary attraction power of granule materials.In addition, due to the presence of liquid film surfactant, when recrystallizing, there is above-mentioned same effect in crystallite of the surfactant again to newly separating out, even if forming crystal brige, also become to be very easy to crush.
The present invention is greatly improved the caking performance of sodium chlorate, surfactant will not be mixed into other production processes, thus few without any harmful effect, anti-caking agent consumption in sour sodium production process to entirely grabbing, optimum addition be a ten thousandth to 3/10000ths, expense is low.
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, with reference to specific embodiment, the present invention is expanded on further.
Embodiment 1
A kind of production technology of anti-caking sodium chlorate, comprises the following steps:
(1) the Crystallization Separation sodium chlorate from sodium chlorate electrolyte, sodium chlorate electrolyte is mixed to get density for 1.30g/cm with appropriate mother liquor3Mixed liquor, sodium chlorate electrolyte be refined brine after electrolysis gained solution, heating in vacuum simultaneously make mixed liquor in 35 DEG C boiling;Wherein, described mother liquor is that the crystallization of sodium chlorate electrolyte is separated out and separates remaining solution after sodium chlorate, the NaCl concentration≤130g/L in mother liquor;Mixed liquor density is 1.50g/cm3When, stop heating;Discharging, cooling, filtering, washing is dried, and obtains sodium chlorate;
(2) sodium chlorate for obtaining step (1), prepare saturation sodium chlorate solution standby, take above-mentioned saturation sodium chlorate solution 500ml, it is placed in beaker, add 2g surfactants, surfactant using fatty glyceride and fatty acid sorbitan mixture, the mass ratio of fatty glyceride and fatty acid sorbitan is 3:2, stirring makes surfactant be dissolved in above-mentioned saturation sodium chlorate solution, adds 500g sodium chlorate crystals, stirs, and stands ten minutes;
(3) by the feed liquid vacuum filtration of step (2), the sodium chlorate crystal that will have been adsorbed surfactant is placed in drying in 12 DEG C of thermostatic drying chambers, and drying time is 2-5h;
(4) dried sodium chlorate is fitted into plastic sample bag, sealing.
Embodiment 2
A kind of production technology of anti-caking sodium chlorate, comprises the following steps:
(1) the Crystallization Separation sodium chlorate from sodium chlorate electrolyte, sodium chlorate electrolyte is mixed to get density for 1.40g/cm with appropriate mother liquor3Mixed liquor, sodium chlorate electrolyte be refined brine after electrolysis gained solution, heating in vacuum simultaneously make mixed liquor in 45 DEG C boiling;Wherein, described mother liquor is that the crystallization of sodium chlorate electrolyte is separated out and separates remaining solution after sodium chlorate, the NaCl concentration≤130g/L in mother liquor;Mixed liquor density is 1.60g/cm3When, stop heating;Discharging, cooling, filtering, washing is dried, and obtains sodium chlorate;
(2) sodium chlorate for obtaining step (1), prepare saturation sodium chlorate solution standby, take above-mentioned saturation sodium chlorate solution 500ml, it is placed in beaker, add 5g surfactants, surfactant using fatty glyceride and fatty acid sorbitan mixture, the mass ratio of fatty glyceride and fatty acid sorbitan is 5:2, stirring makes surfactant be dissolved in above-mentioned saturation sodium chlorate solution, adds 500g sodium chlorate crystals, stirs, and stands ten minutes;
(3) by the feed liquid vacuum filtration of step (2), the sodium chlorate crystal that will have been adsorbed surfactant is placed in drying in 15 DEG C of thermostatic drying chambers, and drying time is 5h;
(4) dried sodium chlorate is fitted into plastic sample bag, sealing.
Embodiment 3
A kind of production technology of anti-caking sodium chlorate, comprises the following steps:
(1) the Crystallization Separation sodium chlorate from sodium chlorate electrolyte, sodium chlorate electrolyte is mixed to get density for 1.35g/cm with appropriate mother liquor3Mixed liquor, sodium chlorate electrolyte be refined brine after electrolysis gained solution, heating in vacuum simultaneously make mixed liquor in 35~45 DEG C boiling;Wherein, described mother liquor is that the crystallization of sodium chlorate electrolyte is separated out and separates remaining solution after sodium chlorate, the NaCl concentration≤130g/L in mother liquor;Mixed liquor density is 1.55g/cm3When, stop heating;Discharging, cooling, filtering, washing is dried, and obtains sodium chlorate;
(2) sodium chlorate for obtaining step (1), prepare saturation sodium chlorate solution standby, take above-mentioned saturation sodium chlorate solution 500ml, it is placed in beaker, add 4g surfactants, surfactant using fatty glyceride and fatty acid sorbitan mixture, the mass ratio of fatty glyceride and fatty acid sorbitan is 4:2, stirring makes surfactant be dissolved in above-mentioned saturation sodium chlorate solution, adds 500g sodium chlorate crystals, stirs, and stands ten minutes;
(3) by the feed liquid vacuum filtration of step (2), the sodium chlorate crystal that will have been adsorbed surfactant is placed in drying in 13 DEG C of thermostatic drying chambers, and drying time is 4h;
(4) dried sodium chlorate is fitted into plastic sample bag, sealing.
The properties of product of embodiment 1-3 such as following table:
Project Sodium chlorate Moisture Water insoluble matter content Proterties after 6 months
Embodiment 1 99.3 0.01 0.006 Quicksand like
Embodiment 2 99.3 0.01 0.006 Quicksand like
Embodiment 3 99.4 0.01 0.005 Quicksand like
Those of ordinary skill in the art should be understood:The discussion of any of the above embodiment is exemplary only, it is not intended that imply that the scope of the present disclosure (including claim) is limited to these examples;Under thinking of the invention, can also be combined between technical characteristic in above example or different embodiments, step can be realized with random order, and there are many other changes of different aspect of the invention as described above, and for simplicity, they are provided not in details.Therefore, all any omission, modification, equivalent, improvement within the spirit and principles in the present invention, made etc., should be included within the scope of the present invention.

Claims (5)

1. a kind of production technology of anti-caking sodium chlorate, it is characterized in that, comprise the following steps:
(1)The Crystallization Separation sodium chlorate from sodium chlorate electrolyte, sodium chlorate electrolyte is mixed to get density for 1.30~1.40g/cm with appropriate mother liquor3Mixed liquor, heating in vacuum simultaneously make mixed liquor in 35~45 DEG C boiling;Wherein, described mother liquor is that the crystallization of sodium chlorate electrolyte is separated out and separates remaining solution after sodium chlorate, the NaCl concentration≤130g/L in mother liquor;Mixed liquor density is 1.50~1.60g/cm3When, stop heating;Discharging, cooling, filtering, washing is dried, and obtains sodium chlorate;
(2)By step(1)The sodium chlorate for obtaining, Prepare saturation sodium chlorate solution standby, take above-mentioned saturation sodium chlorate solution 500ml, be placed in beaker, 2-5g surfactants are added, stirring makes surfactant be dissolved in above-mentioned saturation sodium chlorate solution, 500g sodium chlorate crystals are added, is stirred, stand ten minutes;
(3)By step(2)Feed liquid vacuum filtration, will have been adsorbed surfactant sodium chlorate crystal be placed in 12-15 DEG C of thermostatic drying chamber dry;
(4)Dried sodium chlorate is fitted into plastic sample bag, sealing.
2. a kind of production technology of anti-caking sodium chlorate as claimed in claim 1, it is characterized in that, step(1)In, described sodium chlorate electrolyte is the solution of refined brine gained after electrolysis.
3. a kind of production technology of anti-caking sodium chlorate as claimed in claim 1, it is characterized in that, step(2)In, surfactant is using fatty glyceride and the mixture of fatty acid sorbitan.
4. a kind of production technology of anti-caking sodium chlorate as claimed in claim 3, it is characterized in that, the mass ratio of fatty glyceride and fatty acid sorbitan is(3-5):2.
5. a kind of production technology of anti-caking sodium chlorate as claimed in claim 1, it is characterized in that, step(3)In, drying time is 2-5h.
CN201510831961.1A 2015-11-25 2015-11-25 A kind of production technology of anti-caking sodium chlorate Pending CN106757134A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108560014A (en) * 2018-05-24 2018-09-21 汶川县湘宁氯酸盐有限责任公司 A kind of preparation method of sodium chlorate
CN109972163A (en) * 2019-01-17 2019-07-05 广东鑫国泰科技有限公司 A kind of preparation method of sodium chlorate
EP4105172A1 (en) 2021-06-18 2022-12-21 Nouryon Chemicals International B.V. Anti-caking composition of sodium chlorate

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CA2006611A1 (en) * 1988-12-28 1990-06-28 Carl J. F. Wanngard Process for the reduction of perchlorate in electrolytes used for the production of chlorate
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CN102259839A (en) * 2011-06-17 2011-11-30 德化县新隆泰化工实业有限公司 Anticaking agent special for potassium chlorate

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Publication number Priority date Publication date Assignee Title
CA2006611A1 (en) * 1988-12-28 1990-06-28 Carl J. F. Wanngard Process for the reduction of perchlorate in electrolytes used for the production of chlorate
CN1075469A (en) * 1992-02-21 1993-08-25 福州第一化工厂 Primary crystallization prepares the method for Potcrate
CN1085962A (en) * 1993-05-31 1994-04-27 谭秉彝 The production method of the non-evaporating mother liquor closed cycle of sodium chlorate
CN1099058A (en) * 1994-05-13 1995-02-22 化学工业部大连化工研究设计院 Method for protecting from being crystallization blocked of inorganic salt
CN1319559A (en) * 2001-02-13 2001-10-31 福州一化化学品有限公司 Method for improving blocking-resistant property of sodium chlorate crystal
CN102259839A (en) * 2011-06-17 2011-11-30 德化县新隆泰化工实业有限公司 Anticaking agent special for potassium chlorate

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108560014A (en) * 2018-05-24 2018-09-21 汶川县湘宁氯酸盐有限责任公司 A kind of preparation method of sodium chlorate
CN109972163A (en) * 2019-01-17 2019-07-05 广东鑫国泰科技有限公司 A kind of preparation method of sodium chlorate
CN109972163B (en) * 2019-01-17 2021-02-12 广东鑫国泰科技有限公司 Preparation method of sodium chlorate
EP4105172A1 (en) 2021-06-18 2022-12-21 Nouryon Chemicals International B.V. Anti-caking composition of sodium chlorate

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Application publication date: 20170531