CN1899963A - Method for preparing boric acid from borax - Google Patents
Method for preparing boric acid from borax Download PDFInfo
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- CN1899963A CN1899963A CN 200610047289 CN200610047289A CN1899963A CN 1899963 A CN1899963 A CN 1899963A CN 200610047289 CN200610047289 CN 200610047289 CN 200610047289 A CN200610047289 A CN 200610047289A CN 1899963 A CN1899963 A CN 1899963A
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Abstract
The process of preparing boric acid with borax includes reaction between borax and sulfuric acid or nitric acid of 55-98 % in pH 2.00-3.00 and automatic temperature raise to 70 deg.c for 5-15 min to obtain powdered product; mixing with the saturated boric acid-sodium sulfate solution to solid content of 10-80 %, separating at room temperature in a classifier with introduced air to obtain boric acid in the upper part and sodium sulfate in the lower part; and further separation to obtain boric acid and sodium sulfate or sodium nitrate. Compared with available technology, the present invention has the advantages of simple production process, low cost, no waste liquid exhaust, no corrosion to apparatus and low power consumption.
Description
Technical Field
The invention belongs to the technical field of borate.
Background
Boric acid in China is in increasing demand with the development of industry. At present, boric acid is prepared by a one-step method for decomposing boron ore by sulfuric acid, rich ore is gradually exhausted due to continuous exploitation and utilization, and when boric acid is prepared by a one-step method for lean ore, the amount of mother liquor is large, so that the utilization rate of boron is low, the cost for recovering boric acid and magnesium sulfate in the mother liquor is high, and the boric acid mother liquor is discharged to pollute the environment. So that the neutralization method by utilizing borax and sulfuric acid is the leading position in the industrial boric acid production in China at present. The borax sulfuric acid neutralization method products are boric acid and sodium sulfate. The raw materials are easy to obtain, the process flow is short, the equipment is simple, the process conditions are easy to control, the technology is mature, the consumption of sulfuric acid is low, and the product quality is stable and reliable. So that the boron compound is still commonly adopted by manufacturers at home and abroad (the boron compound production and application is published by the Chengdu science and technology university Press 1992). Boric acid is a relatively weak acid. When strong acid or its salt is used, the boric acid is replaced. The main reaction:
under normal conditions, this is an irreversible reaction, which is fast and quite complete, and is usually carried out in aqueous solution. Their separation is based on solubility characteristics at different temperatures in aqueous solutions. Firstly, the boric acid is crystallized by low temperature cooling, and then the sodium sulfate is separated by high temperature evaporation. And returning the mother liquor after the sodium sulfate is separated out to dissolve borax for circulation, and supplementing a proper amount of water into the solution for dissolving the borax so as to control the concentration of the sodium sulfate not to be too high in order to prevent the sodium sulfate from being eutectoid when cooling and crystallizing the boric acid in the next step. The amount of water added and the amount of mother liquor recycled are two important indicators for the control of the production process. If the operation amount of the two indexes can be reduced in production, the energy consumption can be effectively reduced, and the economic benefit can be obviously improved.
As the technology for producing the boric acid by the borax neutralization method is mature, the production method is improved little so far. The university of Hebei industry and Tianjin university have proposed the technology of improving the production of boric acid by borax neutralization method by using sodium chloride as salting-out agent (Caojilin, etc. the research on the new technology of making boric acid by neutralizing borax with sulfuric acid in Hebei industry university proceedings 2000, 10 months, 29, 5 th period, 37-39 pages). Although the amount of water added is less than that of the traditional process, the amount of evaporating liquid and the amount of cooling liquid are less, the technical route of producing the boric acid by a neutralization method in an aqueous solution is not separated, and the problems of unreasonable energy utilization of heating reaction, cooling separation of the boric acid, heating separation of sodium sulfate and the like still exist.
Disclosure of Invention
The problems existing in the prior art are solved. The invention aims to provide a technical route for producing boric acid by a sulfuric acid neutralization method, which has the advantages of simple process, energy conservation and immediate realization of industrial production.
The technical scheme of the invention is as follows; the reaction product is a mixture of boric acid and sodium sulfate (or sodium nitrate) prepared by neutralizing borax with sulfuric acid or nitric acid, and the boric acid and the sodium sulfate (or sodium nitrate) are separated by utilizing the characteristic that the boric acid is easy to float in saturated liquid containing the boric acid (such as saturated liquid of the boric acid and the sodium sulfate, sodium nitrate, magnesium sulfate, magnesium nitrate or calcium sulfate).
The specific method of the invention is as follows: the preparation process is carried out in two steps, namely reaction and separation:
the first step is as follows: and (2) carrying out neutralization reaction on borax and an inorganic acid (such as sulfuric acid or nitric acid) with the concentration of 55-98% in a reactor with a stirring device for 5-15 min, controlling the pH value of a product to be 2.00-3.00, and automatically raising the temperature of the reaction to about 70 ℃. In this state, the reaction heat continuously evaporates water to keep the inorganic acid at a high concentration, and the reaction can be continued to be complete. The product obtained from the reaction is a mixture of boric acid and sodium sulphate, with a water content of<20%. The reaction products can be stacked for natural cooling and then enter the next procedure, and can also directly enter the next procedure. The second step is that: and (3) carrying out size mixing on the product in the last step by using a saturated solution of boric acid and sodium sulfate (the composition of the saturated solution is unchanged after the temperature is determined according to a phase diagram of the boric acid and the sodium sulfate), so that the solid content of the product is 10-80%, and separating by using gas or saturated solution which does not participate in the reaction as power at normal temperature by utilizing the characteristic that the boric acid is easy to float in the saturated solution. The prepared slurry enters from the middle upper part of the classifier, the gas or saturated liquid which does not participate in the reaction enters from the lower part of the classifier, the boric acid gradually floats on the upper part of the classifier under the push of the gas or saturated liquid which does not participate in the reaction, the sodium sulfate sinks on the lower part of the classifier, and the boric acid and the sodium sulfate are respectively obtained after centrifugal separation. The separator is cylindrical, and the lower part of the separator is a cone with gradually reduced diameter,
the borax used as raw material can be decahydrate, pentahydrate or anhydrous borax, also can be polyborate, rhombic borax ore, soft and hard boron calcium stone ore, also can be used for preparing boric acid from boron magnesium ore, etc. The saturated solution may be, in addition to the above-mentioned boric acid-sodium sulfate: the boric acid-sodium nitrate, boric acid-magnesium sulfate, boric acid-magnesium nitrate or boric acid-calcium sulfate saturated liquid can well separate boric acid from sodium sulfate. The non-reactive gases are air, nitrogen, carbon dioxide and other inert gases.
Compared with the prior art, the invention has the outstanding effects that: 1. simple production process, short flow, less equipment investment, low production cost, realization of directly producing the solid boric acid and high equipment production capacity. 2. The production method is unique, no waste liquid is generated and discharged in the production process, equipment is not corroded, and the environment-friendly effect is good. 3. Because the direct reaction without heating and dissolution and the normal-temperature separation of saturated liquid are adopted, a large amount of energy is saved. The above-mentioned outstanding effect is that prior art can't reach.
Detailed Description
Example 1
1200g of borax is taken and added into a reactor with a stirring device, 200ml of sulfuric acid with 93 percent concentration is added under stirring for reaction for 5 min. During the reaction, the temperature of the reaction materials is automatically increased, the temperature is slowly increased, the reaction speed is accelerated along with the increase of the reaction temperature, and the reaction temperature is rapidly increased and reaches 70 ℃ at the highest. As the temperature increases, the moisture of the reactants evaporates, and the viscosity of the reaction mass decreases. After the reaction, the product was powdery, and 1510g of a powdery material was obtained. The pH value is measured to be 2.73, the water content is 16.99 percent, and the water content is B2O328.91 percent. Sieving the material to obtain three kinds of material with different particle sizes, and measuring water and B2The content of O3 is basically consistent, which indicates that the reactant is very uniform and the reaction effect is very good.
The obtained powder was slurried with a saturated sodium borate sulfate solution to make the solid content 60%. Separation was carried out in a classifier at room temperature: the prepared slurry enters the classifier from the middle upper part of the classifier, air enters the classifier from the lower part of the classifier, boric acid in the material gradually rises and floats on the upper layer of the classifier under the pushing of the air, and sodium sulfate is settled on the lower part of the classifier. Respectively centrifugally separating to obtain boric acid and sodium sulfate. Boric acid meets GB-538-90.
Example 2
1200g of borax is taken and added into a reactor with a stirring device, 200ml of sulfuric acid with 93 percent concentration is added under stirring for reaction for 5 min. The reaction conditions were the same as in example 1. The obtained powdery material is subjected to size mixing by boric acid-sodium sulfate saturated solution, so that the solid content is 30%. And (3) during separation at normal temperature, the slurry enters the classifier from the middle upper part of the classifier, the boric acid-sodium sulfate saturated liquid enters the classifier from the lower part of the classifier, boric acid gradually rises under the push of the saturated liquid and floats on the upper part of the classifier, sodium sulfate is settled to the lower layer of the classifier, and the boric acid and the sodium sulfate are obtained through centrifugal separation respectively.
Example 3
1040g of borax reacted with 173ml of sulfuric acid with a concentration of 93% for 5min with stirring, 1300g of powder with a measured pH of 2.86, a water content of 18.67% and a B content2O328.23 percent. The powder was slurried with a saturated boric acid-sodium sulfate solution to give a solid content of 15%. The pulp enters the classifier from the middle upper part of the classifier at normal temperature, and the air enters the classifier from the classificationThe lower part of the device enters a classifier, boric acid gradually rises and floats on the upper layer of the classifier under the pushing of air, and sodium sulfate is settled on the lower part of the classifier. Respectively centrifugally separating to obtain boric acid and sodium sulfate.
Example 4
1040g of borax reacted with 173ml of sulfuric acid with a concentration of 93% for 5min with stirring, 1300g of powder with a measured pH of 2.86, a water content of 18.67% and a B content2O328.23 percent. The powder was slurried with a saturated boric acid-sodium sulfate solution to give a solid content of 80%. Boric acid and sodium sulfate were separated by the method of example 1.
Example 5
Adding 1800ml of boric acid-sodium sulfate saturated solution into a reactor with a stirring device, adding 500g of borax and 115ml of 93% sulfuric acid under stirring, reacting for 15min, keeping the temperature at about 50 ℃, and cooling to room temperature after the reaction is finished to obtain slurry with the solid content of 40%. Boric acid and sodium sulfate were separated by the method of example 1.
Example 6
1000g of borax is added into a reactor, 170ml of nitric acid with the concentration of 70% is added under stirring, the reaction is carried out for 15min, and the pH value is controlled to be 2.00-3.00. The reaction mixture was made into a slurry containing 30% solids with a saturated solution of boric acid and sodium nitrate. Boric acid and sodium nitrate were isolated by the method of example 1.
Example 7
500g of borax reacts with 176ml of sulfuric acid with the concentration of 65% for 5-10 min under stirring, and the pH value of the obtained powder is 2.25. The following procedure is the same as in example 1.
Example 8
1000g of borax reacts with 270ml of sulfuric acid with the concentration of 80% for 5-10 min under stirring, and the pH value of the obtained powder is 2.26. The following procedure is the same as in example 1.
Claims (6)
1. A method for preparing boric acid by borax is characterized in that the preparation process comprises two steps of reaction and separation, and comprises the following specific steps:
(1) reaction: reacting borax with sulfuric acid or nitric acid with the concentration of 55-98% for 5-15 min in a reactor with a stirring device, controlling the pH value of a product to be 2.00-3.00, automatically heating the reaction to 70 ℃ at most, and obtaining a powdery product after the reaction is finished;
(2) separation: mixing the product with saturated liquid containing boric acid to make the solid content of the product be 10-80%; under normal temperature, slurry enters from the middle upper part of the classifier, gas which does not participate in reaction enters from the lower part of the classifier, and materials are automatically separated under the pushing of the gas: the boric acid floats on the upper part of the classifier, and the sodium sulfate or sodium nitrate sinks on the lower part; respectively centrifugally separating to obtain boric acid and sodium sulfate or sodium nitrate;
wherein: the saturated liquid containing boric acid is a saturated liquid of boric acid-sodium sulfate; the classifier is cylindrical, and the lower part of the classifier is provided with a cone with the diameter gradually reduced; the gas which does not participate in the reaction is air, nitrogen, carbon dioxide and other inert gases.
2. The method for preparing boric acid with borax according to claim 1, wherein the temperature reduction of the reaction product is to naturally reduce the temperature of the product stack, and the water content of the material is less than 20%.
3. The method for preparing the boric acid with the borax according to claim 1, wherein the reaction is carried out in a saturated solution containing the boric acid, the solid content of the reaction reaches 10-80% after the reaction is finished, and the reaction directly enters a classifier for a separation step.
4. The method for preparing the boric acid by the borax according to the claim 1, characterized in that the saturated liquid containing the boric acid enters from the lower part of the classifier in the separation, and the material is automatically classified under the pushing of the saturated liquid.
5. The method for preparing the boric acid by the borax according to the claim 1, 3 or 4, wherein the saturated liquid containing the boric acid is a saturated liquid of boric acid-sodium nitrate, boric acid-magnesium sulfate, boric acid-magnesium nitrate or boric acid-calcium sulfate.
6. The method for preparing the boric acid by the borax according to claim 1, wherein the borax is pentahydrate, decahydrate, anhydrous borax, polyborate, askeite, soft and hard boron calcimine; it is also suitable for preparing boric acid from boron-magnesium ore.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102644090A (en) * | 2012-05-04 | 2012-08-22 | 大连交通大学 | Method for preparing boric acid from crude boron stone through electroosmosis electrolytic method |
| CN103351003A (en) * | 2013-07-23 | 2013-10-16 | 大连理工大学 | Technological method for preparing boric acid, calcium carbonate and sodium nitrate by decomposing ulexite mine with nitric acid |
| CN103771458A (en) * | 2013-09-17 | 2014-05-07 | 西藏金翰投资集团有限公司 | Method for preparing potassium sulfate by using boric acid production raffinate |
| CN104045094A (en) * | 2013-11-13 | 2014-09-17 | 中广核工程有限公司 | Boric acid preparation apparatus used for nuclear power station, and boric acid preparation method thereof |
| CN103708486B (en) * | 2013-11-22 | 2016-01-06 | 南阳东方应用化工研究所 | A kind of method preparing boric acid and SODIUMNITRATE with nitric acid treatment native borax |
| CN105480986A (en) * | 2014-10-15 | 2016-04-13 | 刘浩 | Boric acid preparation method |
| CN106477593A (en) * | 2016-10-12 | 2017-03-08 | 泰誉威（天津）新材料科技有限公司 | A kind of method that boric acid is prepared as raw material with raphite ore deposit |
| CN107311207A (en) * | 2017-06-12 | 2017-11-03 | 沈阳化工大学 | A kind of low-grade magnesite and boron magnesium ore method of comprehensive utilization |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1235070A (en) * | 1998-05-13 | 1999-11-17 | 赵文升 | Washing process for separating magnesium sulphate from boronic acid |
| CN1205120C (en) * | 2003-01-07 | 2005-06-08 | 丹东鑫阳矿业有限公司 | Method for producing magnesium from ludwigite |
| CN100362115C (en) * | 2005-12-06 | 2008-01-16 | 大连市中山区鑫阳矿业化工研究所 | Separation method of boron, magnesium and iron in paigeite |
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2006
- 2006-07-21 CN CNB2006100472898A patent/CN100460322C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102644090A (en) * | 2012-05-04 | 2012-08-22 | 大连交通大学 | Method for preparing boric acid from crude boron stone through electroosmosis electrolytic method |
| CN103351003A (en) * | 2013-07-23 | 2013-10-16 | 大连理工大学 | Technological method for preparing boric acid, calcium carbonate and sodium nitrate by decomposing ulexite mine with nitric acid |
| CN103771458A (en) * | 2013-09-17 | 2014-05-07 | 西藏金翰投资集团有限公司 | Method for preparing potassium sulfate by using boric acid production raffinate |
| CN104045094A (en) * | 2013-11-13 | 2014-09-17 | 中广核工程有限公司 | Boric acid preparation apparatus used for nuclear power station, and boric acid preparation method thereof |
| CN104045094B (en) * | 2013-11-13 | 2018-04-03 | 中广核工程有限公司 | Boron device processed and boron method processed for nuclear power station |
| CN103708486B (en) * | 2013-11-22 | 2016-01-06 | 南阳东方应用化工研究所 | A kind of method preparing boric acid and SODIUMNITRATE with nitric acid treatment native borax |
| CN105480986A (en) * | 2014-10-15 | 2016-04-13 | 刘浩 | Boric acid preparation method |
| CN106477593A (en) * | 2016-10-12 | 2017-03-08 | 泰誉威（天津）新材料科技有限公司 | A kind of method that boric acid is prepared as raw material with raphite ore deposit |
| CN107311207A (en) * | 2017-06-12 | 2017-11-03 | 沈阳化工大学 | A kind of low-grade magnesite and boron magnesium ore method of comprehensive utilization |
| CN107311207B (en) * | 2017-06-12 | 2018-12-18 | 沈阳化工大学 | A kind of low-grade magnesite and boron magnesium ore method of comprehensive utilization |
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| Publication number | Publication date |
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| CN100460322C (en) | 2009-02-11 |
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