CN108159737B - Defoaming agent for wet-process phosphoric acid production and preparation method thereof - Google Patents
Defoaming agent for wet-process phosphoric acid production and preparation method thereof Download PDFInfo
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- CN108159737B CN108159737B CN201711289230.4A CN201711289230A CN108159737B CN 108159737 B CN108159737 B CN 108159737B CN 201711289230 A CN201711289230 A CN 201711289230A CN 108159737 B CN108159737 B CN 108159737B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
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Abstract
The invention discloses a defoaming agent for wet-process phosphoric acid production and a preparation method thereof, wherein the defoaming agent comprises the following raw materials in parts by weight: 10-20 parts of polyether A, 1-5 parts of modified silicon polyether, 0.5-2 parts of active carrier, 1-5 parts of dispersing agent, 5-20 parts of organic solvent and 30-50 parts of deionized water. The defoaming agent prepared by the invention can keep good defoaming and foam inhibiting effects under low concentration and strong acid, and does not influence the quality of phosphoric acid products. The defoaming agent prepared by the invention is not only suitable for wet-process phosphoric acid production, but also suitable for defoaming of strong acid media in mining and other industries.
Description
Technical Field
The invention relates to the technical field of defoaming in wet-process phosphoric acid production, and specifically relates to CO in the wet-process phosphoric acid production process2A stable foam layer defoaming agent formed by continuously dispersing in a reaction liquid and a preparation method thereof.
Background
In the wet-process phosphoric acid production, when the content of carbonate and organic matters in the phosphate rock powder is high, the phosphate rock powder and the acid undergo a chemical reaction to generate a large amount of CO2Gas, CO, as the acidolysis process proceeds violently2The foam layer is continuously dispersed in a reaction liquid containing organic matter components, a stable foam layer with the thickness of 300-700 mm is formed on the surface of an acidolysis tank, and the volume of the foam layer can reach 5-10% of the volume of the reaction liquid. Brings about a plurality of adverse effects on the wet-process phosphoric acid production. Firstly, influence on the separation of powdered rock phosphateThe acidolysis reaction of the dispersant causes the reduction of the production capacity; secondly, the foam layer not only reduces the utilization rate of equipment, but also makes the observation of the liquid level of the material difficult; thirdly, the evaporation of water and the heat removal in the reaction process are hindered, the reaction temperature of the extraction tank is increased, and in severe cases, a great amount of foam is brought to a tail gas absorption system or even overflows the tank, so that P is caused2O5Loss and environmental pollution. Therefore, in the wet-process phosphoric acid production process, a proper amount of defoaming agent must be added to suppress foaming.
The existing defoaming agent in the market mainly comprises tall oil esters, oleic acid and sulfate thereof, fatty acid amide and the like, and the existing defoaming agent has the problems of general defoaming effect and short foam inhibition time in the industrial application of wet-process phosphoric acid production, even increases the viscosity of phosphoric acid production slurry and is not beneficial to the subsequent filtration process treatment. Therefore, the development of the defoaming agent special for wet-process phosphoric acid is important.
Disclosure of Invention
The invention develops a defoaming agent for wet-process phosphoric acid production aiming at the foaming problem in the wet-process phosphoric acid production.
The invention relates to a defoaming agent for wet-process phosphoric acid production and a preparation method thereof; firstly, allyl polyether, hydrogen-containing silicone oil and isopropanol are used for catalytic reaction in chloroplatinic acid to prepare modified silicon polyether, then the modified silicon polyether, polyether A and an active carrier are heated in a proportional reactor to 180-200 ℃ for curing for half an hour, finally, a dispersing agent, a solvent and deionized water are added according to a certain proportion, and a finished product of the defoaming agent is obtained after uniform mixing.
The components and contents (by weight) of the defoaming agent in the invention are as follows:
wherein the structural formula of the polyether A is as follows:
in the above formula, x: y: z: 2: 2: polyether A has a molecular weight of 2000-2800, and a hydroxyl value: 50-60 mgKOH/g;
the active carrier is stearate;
the modified silicon polyether is prepared by the following method:
the method comprises the following steps of (1) mixing allyl polyether, hydrogen-containing silicone oil and isopropanol in a mass ratio of 5-10: 2: 0.5-1, and carrying out chloroplatinic acid catalytic reaction at 100-125 ℃ for 2-8 h to obtain the catalyst; wherein the allyl polyether has a structural formula of CH2＝CHCH2O(PO)m(EO)nCH2(CHCH2) O, molecular weight of 500-1500, EO: PO 2-1: 1, the hydrogen content of the hydrogen-containing silicone oil is 1.5-2%.
Among them, magnesium stearate is preferred as the active carrier.
Wherein, the organic solvent is preferably one or a mixture of methanol, ethanol, propylene glycol and ethylene glycol.
Wherein, the dispersing agent is preferably one or a mixture of several of sodium lignosulfonate, dioctyl sodium sulfosuccinate, coconut oil fatty acid diethanolamide or sodium methylene dinaphthalene sulfonate.
The preparation method of the defoaming agent for wet-process phosphoric acid production comprises the following steps:
1) adding allyl polyether, hydrogen-containing silicone oil and isopropanol into a closed reactor, adding a catalyst chloroplatinic acid under stirring, repeatedly replacing nitrogen in the reactor, controlling the water content and oxygen content of the reactor to be less than 30ppm, heating to 100-125 ℃, reacting for 2-8 hours, and preserving heat for later use; wherein the mass ratio of the allyl polyether to the hydrogen-containing silicone oil to the isopropanol is 5-10: 2: 0.5 to 1; wherein the allyl polyether has a structural formula of CH2＝CHCH2O(PO)m(EO)nCH2(CHCH2) O, molecular weight of 500-1500, EO: PO 2-1: 1, the hydrogen content of the hydrogen-containing silicone oil is 1.5-2%;
2) preparing a defoaming agent: adding polyether A and an active carrier into the modified silicon polyether obtained in the step 1) in proportion, heating to 180-200 ℃, preserving heat, curing, reacting for 0.3-0.7 h, adding a dispersing agent, an organic solvent and deionized water into a reactor in proportion, continuously stirring uniformly, cooling and discharging to obtain the defoaming agent.
The invention has the technical characteristics that: the product is prepared by adopting a synthesis process under normal pressure, and the foam inhibition capability of the defoaming agent can be improved through the curing action of the active carrier, the polyether A and the modified silicon polyether at high temperature. The invention adopts the dispersing agent such as coconut oil fatty acid diethanolamide and the like to effectively improve the dispersing capacity of the defoaming agent in the ore pulp, and greatly improve the defoaming speed of the defoaming agent under the combined action of the dispersing agent and the organic solvent. Aiming at the problem that a large amount of foam is generated in wet-process phosphoric acid production, the defoaming agent prepared by the method has strong defoaming performance and has a good foam inhibition performance.
Detailed Description
Example 1
Preparing a defoaming agent: adding 6g of allyl polyether (molecular weight is 1200, wherein EO: PO is 1: 1) into a closed reactor, adding 2g of hydrogen-containing silicone oil (hydrogen content is 1.6%) and 1g of isopropanol, adding chloroplatinic acid serving as a catalyst, repeatedly replacing nitrogen in the reactor, stirring, heating to 120 ℃ to react for 3 hours, adding 3g of magnesium stearate and 50g of polyether A (molecular weight is 2100, hydroxyl value is 50-60 mgKOH/g), keeping the temperature, curing for 0.5 hour, adding 6g of coconut oil fatty acid diethanolamide, 30g of ethanol and 60g of water into the reactor, continuously stirring uniformly, and finally cooling and discharging to obtain the defoaming agent I.
Example 2
Preparing a defoaming agent: adding 6g of allyl polyether (molecular weight is 800, wherein EO: PO is 1: 1) into a closed reactor, adding 2g of hydrogen-containing silicone oil (hydrogen content is 1.6%) and 1g of isopropanol, adding a catalyst chloroplatinic acid, repeatedly replacing nitrogen in the reactor, stirring, heating to 115 ℃ to react for 2.5 hours, adding 3g of magnesium stearate and 50g of polyether A (molecular weight is 2500, hydroxyl value is 50-60 mgKOH/g), keeping the temperature, curing for 0.5 hour, finally adding 6g of coconut oil fatty acid diethanolamide, 30g of ethanol and 60g of water into the reactor, continuously stirring uniformly, and finally cooling and discharging to obtain a defoaming agent II.
Example 3
Preparing a defoaming agent: adding 6g of allyl polyether (molecular weight is 1200, wherein EO: PO is 1: 1) into a closed reactor, adding 2g of hydrogen-containing silicone oil (hydrogen content is 1.6%) and 1g of isopropanol, adding a catalyst chloroplatinic acid, repeatedly replacing nitrogen in the reactor, stirring, heating to 120 ℃ to react for 3 hours, adding 3g of magnesium stearate and 50g of polyether A (molecular weight is 2100, hydroxyl value is 50-60 mgKOH/g), keeping the temperature, curing for 0.5 hour, adding 6g of dioctyl sulfosuccinate sodium salt, 30g of methanol and 60g of water into the reactor, continuously stirring uniformly, and finally cooling and discharging to obtain the defoamer III.
Static defoaming Performance test of defoaming agent
The method comprises the following steps: placing a 500ml measuring cylinder in a constant temperature tank at 78 ℃, keeping the temperature constant, adding 30g of phosphorite slurry, 30ml of 20% diluted phosphoric acid and a proper amount of water, stirring at the rotating speed of 200rpm, dropwise adding 12ml of 93% concentrated sulfuric acid, stopping stirring when the foam volume reaches the maximum, starting a stopwatch, and recording the foam reduction volume every 10 s.
Foam inhibition performance test of defoaming agent
The method comprises the following steps: and (3) placing a 500ml measuring cylinder in a constant temperature tank at 78 ℃ for constant temperature, respectively adding 30g of phosphate rock powder, a certain amount of defoaming agent (blank test without defoaming agent) and 30ml of 20% diluted phosphoric acid, stirring at the rotating speed of 200rpm, dropwise adding 12ml of 93% concentrated sulfuric acid, starting a stopwatch at the same time, and recording the rising volume of the foam every 10 s.
Comparison of the properties of the antifoam examples is shown in tables 1 and 2
TABLE 1 defoaming agent defoaming Performance test
Table 2 shows the foam suppressing performance of the defoaming agent
As can be seen from tables 1 and 2, the defoaming agent provided by the present invention has excellent defoaming and foam suppressing capabilities.
Claims (5)
1. The defoaming agent for wet-process phosphoric acid production is characterized by comprising the following components in parts by weight: 10-20 parts of polyether A, 1-5 parts of modified silicon polyether, 0.5-2 parts of active carrier, 1-5 parts of dispersing agent, 5-20 parts of organic solvent and 30-50 parts of deionized water;
wherein polyether A has the following structural formula:
in the structural formula of the polyether A, x: y: z: 2: 2: 1, its molecular weight is about 2000-2800, hydroxyl value: 50-60 mgKOH/g;
the active carrier is stearate;
the modified silicon polyether is prepared by the following method:
the method comprises the following steps of (1) mixing allyl polyether, hydrogen-containing silicone oil and isopropanol in a mass ratio of 5-10: 2: 0.5-1, and carrying out chloroplatinic acid catalytic reaction at 100-125 ℃ for 2-8 h to obtain the catalyst; wherein the allyl polyether has a structural formula of CH2＝CHCH2O(PO)m(EO)nCH2(CHCH2) O, molecular weight of 500-1500, EO: PO 2-1: 1, the hydrogen content of the hydrogen-containing silicone oil is 1.5-2%.
2. The antifoaming agent for wet process phosphoric acid production according to claim 1, wherein the active carrier is magnesium stearate.
3. The antifoaming agent for wet process phosphoric acid production according to claim 1, wherein the dispersing agent is one or a mixture of sodium lignosulfonate, dioctyl sodium sulfosuccinate, coconut fatty acid diethanolamide and sodium methylene dinaphthalene sulfonate.
4. The antifoaming agent for wet process phosphoric acid production according to claim 1, wherein the organic solvent is one or a mixture of methanol, ethanol, propylene glycol and ethylene glycol.
5. A method for preparing the antifoaming agent for wet process phosphoric acid production according to claim 1, characterized in that:
1) firstly, preparing modified silicon polyether according to the following method: adding allyl polyether, hydrogen-containing silicone oil and isopropanol into a closed reactor, adding a catalyst chloroplatinic acid under stirring, repeatedly replacing nitrogen in the reactor, controlling the water content and oxygen content of the reactor to be less than 30ppm, heating to 100-125 ℃, reacting for 2-8 hours, and preserving heat for later use; wherein the mass ratio of the allyl polyether to the hydrogen-containing silicone oil to the isopropanol is 5-10: 2: 0.5 to 1; wherein the allyl polyether has a structural formula of CH2＝CHCH2O(PO)m(EO)nCH2(CHCH2) O, molecular weight of 500-1500, EO: PO 2-1: 1, the hydrogen content of the hydrogen-containing silicone oil is 1.5-2%;
2) preparing a defoaming agent: adding the modified silicon polyether obtained in the step 1) into the polyether A and the active carrier in proportion, heating to 180-200 ℃, preserving heat, curing and reacting for 0.3-0.7 h, finally adding the dispersing agent, the organic solvent and the deionized water into the reactor in a certain proportion, continuously stirring uniformly, and finally cooling and discharging to obtain the defoaming agent.
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| CN201711289230.4A CN108159737B (en) | 2017-12-07 | 2017-12-07 | Defoaming agent for wet-process phosphoric acid production and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088128A (en) * | 1992-12-14 | 1994-06-22 | 旅顺联营化工厂 | Mighty defoamer |
| CN1299694A (en) * | 2000-11-27 | 2001-06-20 | 张金保 | Defoamer and its preparation |
| CN101637708A (en) * | 2009-09-01 | 2010-02-03 | 陕西科技大学 | Method for preparing solvent-free polyether grafting organosilico/diamide compound emulsion defoamer |
| CN105031978A (en) * | 2015-08-27 | 2015-11-11 | 杭州彤诚新材料技术有限公司 | Silyl ether mixed defoaming agent emulsion and preparation method thereof |
| CN106334349A (en) * | 2016-11-10 | 2017-01-18 | 中海油天津化工研究设计院有限公司 | Antifoaming agent for flue gas desulphurization system and preparing method thereof |
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- 2017-12-07 CN CN201711289230.4A patent/CN108159737B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088128A (en) * | 1992-12-14 | 1994-06-22 | 旅顺联营化工厂 | Mighty defoamer |
| CN1299694A (en) * | 2000-11-27 | 2001-06-20 | 张金保 | Defoamer and its preparation |
| CN101637708A (en) * | 2009-09-01 | 2010-02-03 | 陕西科技大学 | Method for preparing solvent-free polyether grafting organosilico/diamide compound emulsion defoamer |
| CN105031978A (en) * | 2015-08-27 | 2015-11-11 | 杭州彤诚新材料技术有限公司 | Silyl ether mixed defoaming agent emulsion and preparation method thereof |
| CN106334349A (en) * | 2016-11-10 | 2017-01-18 | 中海油天津化工研究设计院有限公司 | Antifoaming agent for flue gas desulphurization system and preparing method thereof |
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