CN101823752A - Method for co-production of hydrochloric acid in preparation of nano barium sulfate by barium chloride - Google Patents

Method for co-production of hydrochloric acid in preparation of nano barium sulfate by barium chloride Download PDF

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Publication number
CN101823752A
CN101823752A CN 201010158936 CN201010158936A CN101823752A CN 101823752 A CN101823752 A CN 101823752A CN 201010158936 CN201010158936 CN 201010158936 CN 201010158936 A CN201010158936 A CN 201010158936A CN 101823752 A CN101823752 A CN 101823752A
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hydrochloric acid
bariumchloride
barium sulfate
nano
nano barium
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CN 201010158936
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王嘉兴
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Abstract

The invention relates to the technical field of packing preparation, in particular to a method for co-production of hydrochloric acid in the preparation of nano barium sulfate by barium chloride. In the main technical scheme, the method comprises the following steps: using barium sulfate to remove impurities after reaction of barium chloride and sulfuric acid, mixing to produce mixed solution of barium sulfate and hydrochloric acid, then using barium chloride to remove impurities, carrying out centrifugation, washing, drying and crushing to obtain the nano barium sulfate, and carrying out vacuum distillation for the filtrate with hydrochloric acid to obtain a hydrochloric acid product of more than 30 percent. The invention has the advantages of simple production process and equipment and low cost, and not only can be used for preparing the target product nano barium sulfate, but also can be used for co-production of the hydrochloric acid product. Therefore, the invention can create high economic value.

Description

A kind of method for preparing nano barium sulfate and co-producing hydrochloric acid with bariumchloride
Technical field
The present invention relates to technical field of filler preparation, especially a kind of method for preparing nano barium sulfate and co-producing hydrochloric acid with bariumchloride.
Background technology
Barite belongs to Nonrenewable resources, is one of trump-cards in the export of mineral products of China, is widely used in the weighting agent of oil, Sweet natural gas drilling mud, and the consumption in fields such as barium chemical industry, fillers is also increasing year by year.China's barite resource is quite abundant, is distributed in the whole nation 21 provinces (district), and 3.6 hundred million tons in total retained reserve ore occupies the 1st in the world.Wherein, barium sulfate is because water insoluble, is insoluble to acid and has following purposes widely:
Raw material or weighting agent as paint, printing ink, plastics, poster paint, makeup, store battery, both make weighting agent in the rubber item, played strengthening action again, made weighting agent and weighting agent in the polychlorostyrene ethane resin, the surface coated agent of photographic pape and art paper, the sizing agent that textile industry is used.Glasswork can play froth breaking and increase the glossy effect as finings.Can be used as the protection walls material that anti-radioactive rays are used.Also be used for industries such as pottery, enamel, spices and pigment.Also be the raw material material of making other barium salts---powder coating, paint, priming paint peculiar to vessel, armament equipment lacquer, automobile finish, emulsion paint, interior outer wall building coating, can improve that product is fast light, weather-proof, chemically-resistant and electrochemical corrosion and product decoration effect, strengthen the resistance to impact shock of coating.Inorganic industry is as the raw material of making other barium salts such as hydrated barta, barium carbonate, bariumchloride etc.Be used for bottoming and modulation printing paint vehicle during timber industry production grain printing plate.In the organic synthesis as phthalocyanine and color lake production physique filler.
The preparation method of tradition barium sulfate is: is mixed with the saltcake solution that adds after removing calcium, magnesium by barium sulfide solution, react in 80 ℃, generate and precipitate, after suction filtration, washing and pickling, adjusting pH value 5~6 refilters, drying, and pulverizing makes.
For example application number is 02135370.0 to disclose a kind of preparation method of nano barium sulfate, is to utilize complexometry to prepare nanometer BaSO 4Method.Mainly be made up of complex reaction and two steps of precipitin reaction, the concrete step is poly-as follows: (A) with Ba 2+Solution and EDTA enveloping agent solution place reactor that complex reaction takes place, and utilize ammoniacal liquor regulation system pH, Ba under the agitation condition 2+Has certain stable BaY with complexing agent EDTA reaction generation 2-Complexing is (B) with (A) gained complex compound BaY 2-Solution and SO 4 2-Precipitin reaction takes place down and is prepared into nano level BaSO in solution reaction, agitation condition 4Particle.Adopt the prepared nano barium sulfate product of the present invention to be blue light for hexagonal crystal shape, median size 25nm, size-grade distribution 20~40nm.But prior art all also exists complex manufacturing, production unit is huge, cost is higher drawback, and barium slag also of no use at present prepares the relevant report of the method for process white co-production of hydrochloric.
Summary of the invention
At above-mentioned the deficiencies in the prior art, the object of the present invention is to provide the method for a kind of production technique and equipment nano barium sulfate and co-producing hydrochloric acid simple, with low cost.
To achieve these goals, technical scheme of the present invention is as follows:
A kind ofly prepare the method for nano barium sulfate and co-producing hydrochloric acid with bariumchloride, preparation technology is:
Step 1, earlier that bariumchloride is water-soluble, make that the volumetric concentration of barium chloride solution is 10%~60%, after barium chloride solution being handled with 4%~8% tensio-active agent, the barium chloride solution that tensio-active agent was handled is injected in the reactor to stockline by bariumchloride then again;
Step 2, will dissolve good aqueous sodium persulfate solution and give the stockline injecting reactor by sodium sulfate, wherein bariumchloride in the reactor and sodium sulfate are 1: 0.27~0.67 by the mass ratio of pure substance; Simultaneously the stirrer in the reactor evenly stirs with 300~500 rev/mins rotating speed, and chemical reaction obtains the mixing liquid of barium sulfate and hydrochloric acid, mixing liquid through whizzer filter filter cake and filtrate;
Step 3, filter cake carry out drying and pulverizing by drying machine, pulverizer drying successively after washing, be packaged to be the nano barium sulfate product;
Step 4, filtrate obtain hydrochloric acid through underpressure distillation.
Tensio-active agent in the described step 1 is the one or more combination thing in the cruel coupling agent of phthalandione, stearic acid or the xylogen.
Bariumchloride in the described step 1 is that low-grade content is the technical grade bariumchloride more than 90%~100%.
The volumetric concentration of the barium chloride solution in the described step 1 is 25%~34%.
The volumetric concentration of the aqueous sodium persulfate solution in the described step 2 is 15%~50%.
Chemical principle of the present invention is as follows:
BaCl 2+Na 2SO 4=BaSO 4+2NaCl
The present invention utilizes bariumchloride and sodium sulfate reaction to obtain barium sulfate and hydrochloric acid earlier, barium sulfate makes nano barium sulfate through super-dry, pulverizing, simple, the easy row of cost production technique of the present invention and equipment thereof, not only can prepare the target product nano barium sulfate, go back the co-production of hydrochloric product simultaneously, and the productive rate of salt acid product is more than 30%; Because the preparation raw material is low-grade bariumchloride, it is with low cost, so the present invention can create very high economic worth.
Description of drawings
Fig. 1 is a process flow diagram of the present invention;
Wherein:
The 1-reactor, the 2-whizzer, the 3-drying machine, the 4-pulverizer, the 5-bariumchloride is given stockline, and 6-sodium sulfate is given stockline.
Embodiment
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described in further detail.
Embodiment 1
A kind ofly prepare the method for nano barium sulfate and co-producing hydrochloric acid with bariumchloride, preparation technology is:
Earlier 400 kilograms of bariumchlorides of the technical grade of low-grade content more than 90% are dissolved in 11080 kg of water, with being injected in the reactor for stockline 5 by bariumchloride after the cruel coupling agent treatment of 4% phthalandione; It is good to dissolve again, and volumetric concentration is that 50% sodium sulfate is given stockline 6 injecting reactors 1 by sodium sulfate, and wherein bariumchloride in the reactor and sodium sulfate are 1: 0.38 by the mass ratio of pure substance; Evenly stir with 300 rev/mins rotating speed then, chemical reaction obtains the mixing liquid of barium sulfate and hydrochloric acid; Mixing liquid through whizzer 2 filter filter cake and filtrate, filter cake through the washing after carry out drying and pulverizing by drying machine 3, pulverizer 4 dryings successively, be packaged to be 312.2 kilograms of nano barium sulfate products; Described filtrate obtains 156.55 kilograms of hydrochloric acid through underpressure distillation.
Embodiment 2
A kind ofly prepare the method for nano barium sulfate and co-producing hydrochloric acid with bariumchloride, preparation technology is:
Earlier 400 kilograms of bariumchlorides of the technical grade of low-grade content more than 90% are dissolved in 2770 kg of water, handle the back with 3% xylogen and be injected in the reactor for stockline 5 by bariumchloride; It is good to dissolve again, and volumetric concentration is that 32% sodium sulfate is given stockline 6 injecting reactors 1 by sodium sulfate, and wherein bariumchloride in the reactor and sodium sulfate are 1: 0.58 by the mass ratio of pure substance; Evenly stir with 400 rev/mins rotating speed then, chemical reaction obtains the mixing liquid of barium sulfate and hydrochloric acid; Mixing liquid through whizzer 2 filter filter cake and filtrate, filter cake through the washing after carry out drying and pulverizing by drying machine 3, pulverizer 4 dryings successively, be packaged to be 558.7 kilograms of nano barium sulfate products; Described filtrate obtains 780.14 kilograms of hydrochloric acid through underpressure distillation.
Embodiment 3
A kind ofly prepare the method for nano barium sulfate and co-producing hydrochloric acid, it is characterized in that preparation technology is with bariumchloride:
Earlier 400 kilograms of bariumchlorides of the technical grade of low-grade content more than 90% are dissolved in 2216 kg of water, handle the back with 8% tensio-active agent (wherein stearic acid 1%, xylogen 7%) and be injected in the reactor for stockline 5 by bariumchloride; It is good to dissolve again, and volumetric concentration is that 15% sodium sulfate is given stockline 6 injecting reactors 1 by sodium sulfate, and wherein bariumchloride in the reactor and sodium sulfate are 1: 0.67 by the mass ratio of pure substance; Evenly stir with 500 rev/mins rotating speed then, chemical reaction obtains the mixing liquid of barium sulfate and hydrochloric acid; Mixing liquid through whizzer 2 filter filter cake and filtrate, filter cake through the washing after carry out drying and pulverizing by drying machine 3, pulverizer 4 dryings successively, be packaged to be 560.1 kilograms of nano barium sulfate products; Described filtrate obtains 403.73 kilograms of hydrochloric acid through underpressure distillation.
The foregoing description is preferred embodiment of the present invention, is not to be used for limiting the scope of the present invention, so all equivalences of being done with described feature of claim of the present invention and principle change or modify, all should be included within the claim scope of the present invention.
After testing, prepared and the every index such as the table 1 of process white.
Table 1: the detection data of process white
Project The nano barium sulfate index The embodiment of the invention 1 The embodiment of the invention 1 The embodiment of the invention 1
Barium sulfate ??≥98.0% ?99.23% ??99.01% ??98.75%
The water solubles ??≤0.30% ?0.20% ??0.19% ??0.29%
Iron (in Fe) ??≤0.006% ?0.005% ??0.004% ??0.004%
The pH value ??6.5~9.0 ?8.7 ??6.8 ??6.9
Whiteness ??≥92% ?97% ??97% ??96%
Moisture ??≤0.30% ?0.25% ??0.25% ??0.26%
Oil number ??10~30g/100g ?22g/100g ??17g/100g ??20g/100g
??D50 ??0.6um ?0.6um ??0.6um ??0.6um
??D100 ??2um ?2um ??2um ??2um
As can be seen from the above table, the barium sulfate that utilizes the present invention to produce is the Nano grade product.

Claims (5)

1. one kind prepares the method for nano barium sulfate and co-producing hydrochloric acid with bariumchloride, it is characterized in that preparation technology is:
Step 1, earlier that bariumchloride is water-soluble, make that the volumetric concentration of barium chloride solution is 10%~60%, after barium chloride solution being handled with 4%~8% tensio-active agent, the barium chloride solution that tensio-active agent was handled is injected in the reactor to stockline by bariumchloride then again;
Step 2, will dissolve good aqueous sodium persulfate solution and give the stockline injecting reactor by sodium sulfate, wherein bariumchloride in the reactor and sodium sulfate are 1: 0.27~0.67 by the mass ratio of pure substance; Simultaneously the stirrer in the reactor evenly stirs with 300~500 rev/mins rotating speed, and chemical reaction obtains the mixing liquid of barium sulfate and hydrochloric acid, mixing liquid through whizzer filter filter cake and filtrate;
Step 3, filter cake carry out drying and pulverizing by drying machine, pulverizer drying successively after washing, be packaged to be the nano barium sulfate product;
Step 4, filtrate obtain hydrochloric acid through underpressure distillation.
2. according to claim 1ly prepare the method for nano barium sulfate and co-producing hydrochloric acid with bariumchloride, it is characterized in that: the tensio-active agent in the described step 1 is the one or more combination thing in the cruel coupling agent of phthalandione, stearic acid or the xylogen.
3. according to claim 1ly prepare the method for nano barium sulfate and co-producing hydrochloric acid with bariumchloride, it is characterized in that: the bariumchloride in the described step 1 is that low-grade content is the technical grade bariumchloride more than 90%~100%.
4. according to claim 1ly prepare the method for nano barium sulfate and co-producing hydrochloric acid with bariumchloride, it is characterized in that: the volumetric concentration of the barium chloride solution in the described step 1 is 25%~34%.
5. according to claim 1ly prepare the method for nano barium sulfate and co-producing hydrochloric acid with bariumchloride, it is characterized in that: the volumetric concentration of the aqueous sodium persulfate solution in the described step 2 is 15%~50%.
CN 201010158936 2009-04-13 2010-03-24 Method for co-production of hydrochloric acid in preparation of nano barium sulfate by barium chloride Pending CN101823752A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102167386A (en) * 2011-03-16 2011-08-31 清华大学 Method for preparing barium sulfate nanoparticles
CN111574853A (en) * 2020-06-09 2020-08-25 江苏群鑫粉体科技股份有限公司 Modified barium sulfate for heavy-duty anticorrosive paint
CN112299467A (en) * 2019-07-31 2021-02-02 北京化工大学 Preparation method of monodisperse oil phase nano barium sulfate dispersoid

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101638241A (en) * 2009-04-13 2010-02-03 王嘉兴 Method for preparing nano-barium sulfate coproducing sodium chloride

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101638241A (en) * 2009-04-13 2010-02-03 王嘉兴 Method for preparing nano-barium sulfate coproducing sodium chloride

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
《太原工业大学学报》 19890930 王振汗等 以硝板和黑灰为原料研制沉淀硫酸钡 第9~16页 1-5 第20卷, 第3期 2 *
《高校化学工程学报》 20050430 王敏等 纳米硫酸钡制备过程中的蒸馏法破乳和微孔液的循环使用 第187~191页 1-5 第19卷, 第2期 2 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102167386A (en) * 2011-03-16 2011-08-31 清华大学 Method for preparing barium sulfate nanoparticles
CN102167386B (en) * 2011-03-16 2013-07-03 清华大学 Method for preparing barium sulfate nanoparticles
CN112299467A (en) * 2019-07-31 2021-02-02 北京化工大学 Preparation method of monodisperse oil phase nano barium sulfate dispersoid
CN112299467B (en) * 2019-07-31 2022-10-28 北京化工大学 Preparation method of monodisperse oil-phase nano barium sulfate dispersoid
CN111574853A (en) * 2020-06-09 2020-08-25 江苏群鑫粉体科技股份有限公司 Modified barium sulfate for heavy-duty anticorrosive paint

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Address after: 523000, room five, building 508, Jinhai building, Dongcheng District Tong Road, Dongguan, Guangdong

Applicant after: Wang Jiaxing

Address before: Wushi Village Primary School in Dongguan city of Dongcheng District province Guangdong road 523000 Lane 1 No. 6 main mountain

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Application publication date: 20100908