CN102963971A - Method for recycling potassium chloride and organisms from initiator production waste liquid - Google Patents
Method for recycling potassium chloride and organisms from initiator production waste liquid Download PDFInfo
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- CN102963971A CN102963971A CN2012104716990A CN201210471699A CN102963971A CN 102963971 A CN102963971 A CN 102963971A CN 2012104716990 A CN2012104716990 A CN 2012104716990A CN 201210471699 A CN201210471699 A CN 201210471699A CN 102963971 A CN102963971 A CN 102963971A
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Abstract
The invention relates to the technical field of initiator production waste liquid recycling, and particularly relates to a method for recycling potassium chloride and organisms from the initiator production waste liquid. The method comprises the following steps of: (I) adding the collected initiator production waste liquid into a glass reaction kettle; and (II) starting a stirrer to stir, adding hydrochloric acid into the glass reaction kettle to conduct a neutralization reaction with the initiator production waste liquid; and when the pH value of the initiator production waste liquid reaches 6.5-7.5, stopping stirring, and standing for 1-2 hours until the initiator production waste liquid is divided into an upper layer and a lower layer. According to the invention, hydrochloric acid is added into the initiator production waste liquid to conduct a neutralization reaction and the reaction liquid is divided into an upper layer and a lower layer after the neutralization reaction, wherein the upper layer consists of organisms, and the aqueous phase containing potassium chloride on the lower layer is evaporated, separated and dried to obtain potassium chloride; and the method provided by the invention has the characteristics of stability and reliability, environmental protection, high recovery rate of potassium chloride and organisms and high purity of potassium chloride, reduces the production cost and avoids resource waste.
Description
Technical field
The present invention relates to initiator and produce waste liquid recovery technology field, is that a kind of production from initiator reclaimed Repone K and organic method the waste liquid.
Background technology
In the new certain herbaceous plants with big flowers tert-butyl acrylate of initiator peroxidation, the new certain herbaceous plants with big flowers acid of peroxidation isopropyl benzene ester synthesis process, can produce a large amount of waste liquids, the main component of waste liquid is the Repone K of by-product and the organic raw material that does not react completely (being mainly tertbutyl peroxide and isopropyl benzene hydroperoxide), the new certain herbaceous plants with big flowers acid of the new certain herbaceous plants with big flowers tert-butyl acrylate of one ton of peroxidation of every production or peroxidation isopropyl phenyl ester product will produce about one ton of waste liquid, contain 200kg to 250kg Repone K in the waste liquid per ton, 60kg to 120kg organism.Usually waste liquid is entered Sewage treatment systems at present, not only environment is brought disadvantageous effect, and wasted Repone K resource in short supply.
Summary of the invention
The invention provides a kind of production from initiator and reclaim Repone K and organic method the waste liquid, overcome the deficiency of above-mentioned prior art, it can solve effectively that the new certain herbaceous plants with big flowers acid of the new certain herbaceous plants with big flowers tert-butyl acrylate of initiator peroxidation, peroxidation isopropyl phenyl ester produces that waste liquid directly enters Sewage treatment systems and the problem that causes environmental pollution and the wasting of resources.
Technical scheme of the present invention realizes by following measures: a kind of production from initiator reclaimed Repone K and organic method the waste liquid, carry out in the steps below: the first step, and the initiator of collecting is produced waste liquid add in the glass reaction still; Second step, the unlatching stirrer stirs, hydrochloric acid joined in the glass reaction still produce waste liquid with initiator and carry out neutralization reaction, after reaching 6.5 to 7.5, the pH value that makes initiator produce waste liquid stops to stir, after leaving standstill 1 hour to 2 hours, initiator production waste liquid is divided into two-layer up and down, and the upper strata is oil phase, and lower floor is the water of chloride containing potassium; The 3rd step, it is to evaporate in 100 ℃ to 105 ℃ the evaporative crystallizer that the water of lower floor's chloride containing potassium is placed on temperature, being evaporated to Repone K is 30% to 38% at the mass percent of aqueous phase, then obtained solid phase in 5 minutes to 10 minutes with the whizzer centrifugation after being cooled to normal temperature, solid phase obtains Repone K after drying; Upper oil phase is organism.
The below is the further optimization and/or improvements to the foregoing invention technical scheme:
It is that the new certain herbaceous plants with big flowers tert-butyl acrylate of peroxidation is produced waste liquid or the new certain herbaceous plants with big flowers acid of peroxidation isopropyl phenyl ester is produced waste liquid that above-mentioned initiator is produced waste liquid.
The rotating speed of above-mentioned whizzer is 1500 rev/mins to 3000 rev/mins.
Above-mentioned drying temperature is 100 ℃ to 120 ℃, and be 4 hours to 8 hours time of drying.
The mass percent of above-mentioned hydrochloric acid is 28% to 35%.
Above-mentioned normal temperature temperature is 25 ℃ to 35 ℃.
The present invention adds hydrochloric acid generation neutralization reaction by producing at initiator in the waste liquid, two-layer about being divided into after the neutralization reaction, the upper strata is organism, and the water of lower floor's chloride containing potassium obtains Repone K through evaporation, separation and drying; Have the high characteristics of Repone K purity that reliable and stable, environmental protection, Repone K and the organic rate of recovery are high, obtain, reduced production cost, stopped the wasting of resources.
Embodiment
The present invention is not subjected to the restriction of following embodiment, can determine concrete embodiment according to technical scheme of the present invention and practical situation.
Embodiment 1, should produce from initiator and reclaim Repone K and organic method the waste liquid, carries out in the steps below: the first step, and the initiator of collecting is produced waste liquid add in the glass reaction still; Second step, the unlatching stirrer stirs, hydrochloric acid joined in the glass reaction still produce waste liquid with initiator and carry out neutralization reaction, after reaching 6.5 to 7.5, the pH value that makes initiator produce waste liquid stops to stir, after leaving standstill 1 hour to 2 hours, initiator production waste liquid is divided into two-layer up and down, and the upper strata is oil phase, and lower floor is the water of chloride containing potassium; The 3rd step, it is to evaporate in 100 ℃ to 105 ℃ the evaporative crystallizer that the water of lower floor's chloride containing potassium is placed on temperature, being evaporated to Repone K is 30% to 38% at the mass percent of aqueous phase, then obtained solid phase in 5 minutes to 10 minutes with the whizzer centrifugation after being cooled to normal temperature, solid phase obtains Repone K after drying; Upper oil phase is organism.With the organism that the obtains plastic barrel of packing into.Be under 100 ℃ to 105 ℃ in temperature, when Repone K was 30% to 38% at the mass percent of aqueous phase, this moment, Repone K was in critical state of saturation at aqueous phase.
Embodiment 2, should produce from initiator and reclaim Repone K and organic method the waste liquid, carry out in the steps below: the first step, and the initiator of collecting is produced waste liquid add in the glass reaction still; Second step, the unlatching stirrer stirs, hydrochloric acid joined in the glass reaction still produce waste liquid with initiator and carry out neutralization reaction, after reaching 6.5 to 7.5, the pH value that makes initiator produce waste liquid stops to stir, after leaving standstill 1 hour or 2 hours, initiator production waste liquid is divided into two-layer up and down, and the upper strata is oil phase, and lower floor is the water of chloride containing potassium; The 3rd step, the water of lower floor's chloride containing potassium is placed in the evaporative crystallizer that temperature is 100 ℃ or 105 ℃ evaporates, being evaporated to Repone K is 30% or 38% at the mass percent of aqueous phase, then obtained solid phase in 5 minutes to 10 minutes with the whizzer centrifugation after being cooled to normal temperature, solid phase obtains Repone K after drying; Upper oil phase is organism.With the organism that the obtains plastic barrel of packing into.Be under 100 ℃ or 105 ℃ in temperature, when Repone K was 30% or 38% at the mass percent of aqueous phase, this moment, Repone K was in critical state of saturation at aqueous phase.
Embodiment 3, and as the optimization of above-described embodiment: it is that the new certain herbaceous plants with big flowers tert-butyl acrylate of peroxidation is produced waste liquid that initiator is produced waste liquid; Perhaps initiator production waste liquid is that the new certain herbaceous plants with big flowers acid of peroxidation isopropyl phenyl ester is produced waste liquid.
Embodiment 4, and as the optimization of above-described embodiment: the rotating speed of whizzer is 1500 rev/mins to 3000 rev/mins.
Embodiment 5, and as the optimization of above-described embodiment: drying temperature is 100 ℃ to 120 ℃, and be 4 hours to 8 hours time of drying.
Embodiment 6, and as the optimization of above-described embodiment: the mass percent of hydrochloric acid is 28% to 35%.
Embodiment 7, and as the optimization of above-described embodiment: the normal temperature temperature is 25 ℃ to 35 ℃.
By the Repone K that above-described embodiment obtains, the Repone K average content is greater than 98%, and average moisture content is less than 1.5% in the Repone K; It is tertbutyl peroxide that initiator is produced the organic main component that obtains when waste liquid is the new certain herbaceous plants with big flowers tert-butyl acrylate production of peroxidation waste liquid, and outward appearance is colourless transparent liquid; It is isopropyl benzene hydroperoxide that initiator is produced the organic main component that obtains when waste liquid is the new certain herbaceous plants with big flowers acid of peroxidation isopropyl phenyl ester production waste liquid, and outward appearance is the lightpink transparent liquid.
Above technical characterictic has consisted of embodiments of the invention, and it has stronger adaptability and implementation result, can increase and decrease according to actual needs non-essential technical characterictic, satisfies the demand of different situations.
Claims (10)
1. one kind is reclaimed Repone K and organic method from initiator production waste liquid, it is characterized in that carrying out in the steps below: the first step, and the initiator of collecting is produced waste liquid add in the glass reaction still; Second step, the unlatching stirrer stirs, hydrochloric acid joined in the glass reaction still produce waste liquid with initiator and carry out neutralization reaction, after reaching 6.5 to 7.5, the pH value that makes initiator produce waste liquid stops to stir, after leaving standstill 1 hour to 2 hours, initiator production waste liquid is divided into two-layer up and down, and the upper strata is oil phase, and lower floor is the water of chloride containing potassium; The 3rd step, it is to evaporate in 100 ℃ to 105 ℃ the evaporative crystallizer that the water of lower floor's chloride containing potassium is placed on temperature, being evaporated to Repone K is 30% to 38% at the mass percent of aqueous phase, then obtained solid phase in 5 minutes to 10 minutes with the whizzer centrifugation after being cooled to normal temperature, solid phase obtains Repone K after drying; Upper oil phase is organism.
2. according to claim 1 production from initiator reclaimed Repone K and organic method the waste liquid, it is characterized in that it is that the new certain herbaceous plants with big flowers tert-butyl acrylate of peroxidation is produced waste liquid or the new certain herbaceous plants with big flowers acid of peroxidation isopropyl phenyl ester is produced waste liquid that initiator is produced waste liquid.
3. according to claim 1 and 2 production from initiator reclaimed Repone K and organic method the waste liquid, and the rotating speed that it is characterized in that whizzer is 1500 rev/mins to 3000 rev/mins.
4. according to claim 1 and 2 production from initiator reclaimed Repone K and organic method the waste liquid, it is characterized in that drying temperature is 100 ℃ to 120 ℃, and be 4 hours to 8 hours time of drying.
5. according to claim 3 production from initiator reclaimed Repone K and organic method the waste liquid, it is characterized in that drying temperature is 100 ℃ to 120 ℃, and be 4 hours to 8 hours time of drying.
6. according to claim 1 and 2 production from initiator reclaimed Repone K and organic method the waste liquid, and the mass percent that it is characterized in that hydrochloric acid is 28% to 35%.
7. according to claim 3 production from initiator reclaimed Repone K and organic method the waste liquid, and the mass percent that it is characterized in that hydrochloric acid is 28% to 35%.
8. according to claim 4 production from initiator reclaimed Repone K and organic method the waste liquid, and the mass percent that it is characterized in that hydrochloric acid is 28% to 35%.
9. according to claim 5 production from initiator reclaimed Repone K and organic method the waste liquid, and the mass percent that it is characterized in that hydrochloric acid is 28% to 35%.
According to claim 1 in 9 described the production from initiator of any one reclaim Repone K and organic method the waste liquid, it is characterized in that the normal temperature temperature is 25 ℃ to 35 ℃.
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| CN201210471699.0A CN102963971B (en) | 2012-11-20 | 2012-11-20 | Method for recycling potassium chloride and organisms from initiator production waste liquid |
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| CN201210471699.0A CN102963971B (en) | 2012-11-20 | 2012-11-20 | Method for recycling potassium chloride and organisms from initiator production waste liquid |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104402788A (en) * | 2014-11-03 | 2015-03-11 | 乌鲁木齐市华泰隆化学助剂有限公司 | Method for recovering and using tert-butyl hydroperoxide from initiator waste liquid |
| CN109019635A (en) * | 2018-07-31 | 2018-12-18 | 南京格洛特环境工程股份有限公司 | Waste liquor treatment process |
| CN113292472A (en) * | 2021-05-26 | 2021-08-24 | 常熟市滨江化工有限公司 | Recycling treatment method for dialkyl peroxide-white carbon black waste |
| CN113290024A (en) * | 2021-05-26 | 2021-08-24 | 常熟市滨江化工有限公司 | Resource recycling treatment method for organic peroxide-calcium carbonate waste |
| CN113382968A (en) * | 2019-01-31 | 2021-09-10 | 诺力昂化学品国际有限公司 | Process for producing salts from aqueous waste streams of organic peroxide production |
| JP2022518845A (en) * | 2019-01-31 | 2022-03-16 | ヌーリオン ケミカルズ インターナショナル ベスローテン フェノーツハップ | How to make salt from aqueous waste logistics of organic peroxide production |
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| US4274969A (en) * | 1978-11-14 | 1981-06-23 | Produits Chimiques Ugine Kuhlmann | Process for treating waste water from propylene oxidation plants |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104402788A (en) * | 2014-11-03 | 2015-03-11 | 乌鲁木齐市华泰隆化学助剂有限公司 | Method for recovering and using tert-butyl hydroperoxide from initiator waste liquid |
| CN109019635A (en) * | 2018-07-31 | 2018-12-18 | 南京格洛特环境工程股份有限公司 | Waste liquor treatment process |
| CN113382968A (en) * | 2019-01-31 | 2021-09-10 | 诺力昂化学品国际有限公司 | Process for producing salts from aqueous waste streams of organic peroxide production |
| JP2022518845A (en) * | 2019-01-31 | 2022-03-16 | ヌーリオン ケミカルズ インターナショナル ベスローテン フェノーツハップ | How to make salt from aqueous waste logistics of organic peroxide production |
| JP7328340B2 (en) | 2019-01-31 | 2023-08-16 | ヌーリオン ケミカルズ インターナショナル ベスローテン フェノーツハップ | Process for producing salts from aqueous waste streams of organic peroxide production |
| TWI831913B (en) * | 2019-01-31 | 2024-02-11 | 荷蘭商諾力昂化學國際股份有限公司 | Process for producing salt from waste streams |
| CN113292472A (en) * | 2021-05-26 | 2021-08-24 | 常熟市滨江化工有限公司 | Recycling treatment method for dialkyl peroxide-white carbon black waste |
| CN113290024A (en) * | 2021-05-26 | 2021-08-24 | 常熟市滨江化工有限公司 | Resource recycling treatment method for organic peroxide-calcium carbonate waste |
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| CN102963971B (en) | 2014-05-21 |
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