CN102010319B - Method for reclaiming coarse diacid by using dimer acid filtered argil residue water substitution method - Google Patents
Method for reclaiming coarse diacid by using dimer acid filtered argil residue water substitution method Download PDFInfo
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- CN102010319B CN102010319B CN 201010542685 CN201010542685A CN102010319B CN 102010319 B CN102010319 B CN 102010319B CN 201010542685 CN201010542685 CN 201010542685 CN 201010542685 A CN201010542685 A CN 201010542685A CN 102010319 B CN102010319 B CN 102010319B
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- carclazyte
- dimeracid
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Abstract
The invention relates to a method for reclaiming coarse diacid by using a dimer acid filtered argil residue water substitution method. The method comprises the following steps of: 1, quantitative delivery with an auger; 2, slurry preparation from argil residue and hot water; 3, steady-flow and quantitative delivery with a screw pump; 4, direct steam heating and boosting water substitution reaction; 5, standing, settlement and oil-residue separation; and 6, centrifugal dehydration of residue slurry.
Description
Technical field
The present invention relates to a kind of dimeracid and filter the carclazyte pulp water reclaims thick diacid for method method.Belong to the oil chemistry industrial circle.
Background technology
In the dimeracid synthetic reaction process, use the carclazyte of oleic acid weight about 12% as catalyzer, contain 25～35% thick diacid and filter in the clay dregs, the thick disposable words of diacid in the clay dregs, this waste residue not only causes environmental pollution, and follows the wasting of resources.At present, the method for dimeracid manufacturing enterprise hydraulic pressure squeezing commonly used reclaims thick diacid, and this method not only labour intensity is big, and it is low to reclaim yield.The waste residue Residual oil is in 13～16% (thick two acid recovering rate 40～50%).Because thick diacid is very unstable in the useless carclazyte, oxidizing reaction easily takes place, form thickness superoxide and polymkeric substance, cause the rate of recovery of thick diacid to descend, the useless carclazyte shelf-time is more long, and the peroxide value of thick diacid is just more high, and iodine number descends more obvious, show that severe oxidation has taken place thick diacid, cause the rate of recovery of thick diacid to decline to a great extent.Polymerization, acidifying, the useless clay dregs after the filtration will in time reclaim thick diacid, can guarantee quality and the rate of recovery of thick diacid like this.Big in order to solve in the useless clay dregs thick two acid recovery labour intensity; the recovery yield is low; waste residue causes environmental pollution problems; we have invented a kind of dimeracid and have filtered the carclazyte pulp water reclaims thick diacid for method method; this method is pollution-free; the production technique cleaning; waste residue Residual oil low (residual 5～6%); thick two acid recovering rate height (rate of recovery is up to more than 80%), the technology cost is low, and labour intensity is little; continuous mechanized operation; the thick diacid that reclaims can be used for preparing the commodity dimeracid, and the carclazyte that removes thick diacid can be used as molding or makes material of construction, or is used for flower culture as acid filling soil of cultivating soil.Also can be further processing regenerated to removing thick diacid carclazyte, circulation re-uses.
Summary of the invention
The present invention is big in order to solve in the useless carclazyte thick two acid recovery labour intensity, and it is low to reclaim yield, and waste residue causes environmental pollution problems, and we have invented a kind of dimeracid and have filtered the carclazyte pulp water and reclaim the method for thick diacid for method, and this method may further comprise the steps:
1, auger is quantitatively carried.
1.1 frequency of delivery is generally controlled at 1～50Hz, preferentially controls at 10～40Hz, especially 20～30Hz;
1.2 operational throughput is generally controlled at 0.01～2m
3/ h preferentially controls at 0.05～1.5m
3/ h, especially 0.2～0.8m
3/ h.
2, clay dregs and hot water are made slurry.
2.1 the weight ratio of clay dregs and hot water is generally controlled 1: 1～5, preferentially controls 1: 1.5～3.5 especially 1: 2～3;
2.2 the hot water temperature generally controls at 50～100 ℃, preferentially controls at 60～98 ℃ especially 85～95 ℃.
3, the spiral pump current stabilization is quantitatively carried.
3.1 feed flow is generally controlled at 0.1～5m3/h, preferentially controls at 0.3～3m3/h, especially 0.5～1.5m3/h;
3.2 transfer pressure is generally controlled at 0.1～1.2Mpa, preferentially controls at 0.3～1Mpa, especially 0.5～0.7MPa.
4, open steam increasing temperature and pressure water is for reaction.
4.1 adopt radio frequency admittance level gauge instrument control bed depth, adopt integration variable valve control input, output flat
4.2 water is generally controlled at 0.1～0.8Mpa for reaction pressure, preferentially controls at 0.3～6Mpa, especially 0.45～0.55MPa;
4.3 open steam pressure is generally controlled at 0.4～1.0Mpa, preferentially controls at 0.5～1Mpa, especially 0.6～0.8MPa;
4.4 water is generally controlled at 50～120n/min for the reaction stirring velocity, preferentially controls at 60～100n/min, especially 80～90n/min;
4.5 water was generally controlled at 10～100min for the reaction times, preferentially controlled at 20～60min, especially 30～40min;
4.6 water is generally controlled at 140～160 ℃ for temperature of reaction, preferentially controls at 145～155 ℃ especially 148～152 ℃.
5, the standing sedimentation dregs of fat separate.
5.1 adopt radio frequency admittance water-oil interface instrument control water-oil interface, adopt integration variable valve control input, the balance of output;
5.2 standing sedimentation dregs of fat separation temperature is generally controlled at 70～100 ℃, preferentially controls at 80～95 ℃ especially 85～90 ℃;
5.3 standing sedimentation dregs of fat disengaging time is generally controlled at 10～60min, preferentially controls at 20～50min, especially 30～35min.
6, slag slurry centrifuge dehydration.
6.1 the slag slurry is by horizontal sedimentation helical-conveyer centrifugal solid-liquid separation, liquid enters process water pond, Gu slag enters the comprehensive utilization manufacturing procedure;
6.2 the water liquid of slag slurry centrifuge dehydration is made the process water of slurry as clay dregs hot water.
Embodiment
Filter clay dregs by the frequency conversion auger with 0.3m
3The operational throughput of/h is balancedly sent to making beating and jar is mixed with 85～95 ℃ technology hot water, makes slurry, and the weight ratio of clay dregs and hot water is controlled at 1: 2, slurry inflow screw rod current stabilization transferpump, and the variable frequency regulating speed control flow is at 0.65m
3/ h, transfer pressure control is at 0.55Mpa, slurry is sent into water for the reactor bottom, open the bottom open steam and heat the sparger valve that boosts, opening water stirs for reactor, control stirring velocity 90n/min, the reactor pressure-stabilisation is at 0.5Mpa, the slurry bed of material is through arriving high-order discharge port behind the 40min, about 150 ℃ of control material temperature keep water for reactor 0.5Mpa, control water for the reactor bed depth by the radio frequency admittance level gauge instrument, open slurry discharging integral control variable valve, make input, output reaches balance.Enter the standing sedimentation separating tank that hot water is housed from water for the mixed liquor tangent line of reactor, because the difference of proportion, thick diacid come-up is accumulated as oil reservoir, by liquid level control output collection slowly, the carclazyte slurry that removes thick diacid progressively is cooled to 90 ℃ in the settling process, open settlement separate jar of slurry discharging integral control variable valve, by radio frequency admittance water-oil interface instrument regulated valve open degree, slurry enters horizontal sedimentation helical-conveyer centrifugal, the hot water circulation of separating is used, and the clay dregs of separation enters the comprehensive utilization operation.
Claims (33)
1. a dimeracid filters the carclazyte pulp water and reclaims the method for thick diacid for method, and this method comprises the steps:
Step 1: auger is quantitatively carried;
Step 2: clay dregs and hot water are made slurry;
Step 3: the spiral pump current stabilization is quantitatively carried;
Step 4: open steam increasing temperature and pressure water is for reaction;
Step 5: the standing sedimentation dregs of fat separate;
Step 6: slag slurry centrifuge dehydration.
2. a kind of dimeracid according to claim 1 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that the auger described in the step 1 quantitatively carries, and adopts the speed control by frequency variation auger quantitatively to carry:
Frequency of delivery control is at 1～50Hz;
Operational throughput control is at 0.01～2m
3/ h.
3. a kind of dimeracid according to claim 2 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that frequency of delivery control is at 10～40Hz.
4. a kind of dimeracid according to claim 2 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that frequency of delivery control is at 20～30Hz.
5. a kind of dimeracid according to claim 2 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that operational throughput control is at 0.05～1.5m
3/ h.
6. a kind of dimeracid according to claim 2 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that operational throughput control is at 0.2～0.8m
3/ h.
7. a kind of dimeracid according to claim 1 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that the clay dregs described in the step 2 and hot water makes slurry:
The weight ratio control of clay dregs and hot water is 1: 1～5;
Hot water temperature's control is at 50～100 ℃.
8. a kind of dimeracid according to claim 7 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that the weight ratio of clay dregs and hot water is controlled 1: 1.5～3.5.
9. a kind of dimeracid according to claim 7 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that the weight ratio of clay dregs and hot water is controlled 1: 2～3.
10. a kind of dimeracid according to claim 7 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that the hot water temperature controls at 60～98 ℃.
11. a kind of dimeracid according to claim 7 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that the hot water temperature controls at 85～95 ℃.
12. a kind of dimeracid according to claim 1 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that the spiral pump current stabilization described in the step 3 quantitatively carries:
Feed flow control is at 0.1～5m
3/ h;
Transfer pressure control is at 0.1～1.2Mpa.
13. a kind of dimeracid according to claim 12 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that feed flow control is at 0.3～3m
3/ h.
14. a kind of dimeracid according to claim 12 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that feed flow control is at 0.5～1.5m
3/ h.
15. a kind of dimeracid according to claim 12 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that transfer pressure control is at 0.3～1Mpa.
16. a kind of dimeracid according to claim 12 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that transfer pressure control is at 0.5～0.7Mpa.
17. a kind of dimeracid according to claim 1 filters the carclazyte pulp water reclaims thick diacid for method method, it is characterized in that the open steam increasing temperature and pressure water described in the step 4 is for reaction: adopt radio frequency admittance level gauge instrument control bed depth, adopt integration variable valve control input, the balance of output;
Water is controlled at 0.1～0.8Mpa for reaction pressure;
The open steam pressure-controlling is at 0.4～1.0Mpa; Water is controlled at 50～120n/min for the reaction stirring velocity;
Water was controlled at 10～100min for the reaction times;
Water is controlled at 140～160 ℃ for temperature of reaction.
18. a kind of dimeracid according to claim 17 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that water for reaction pressure control at 0.3～6Mpa.
19. a kind of dimeracid according to claim 17 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that water for reaction pressure control at 0.45～0.55MPa.
20. a kind of dimeracid according to claim 17 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that the open steam pressure-controlling is at 0.5～1Mpa.
21. a kind of dimeracid according to claim 17 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that the open steam pressure-controlling is at 0.6～0.8Mpa.
22. a kind of dimeracid according to claim 17 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that water for the control of reaction stirring velocity at 60～100n/min.
23. a kind of dimeracid according to claim 17 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that water for the control of reaction stirring velocity at 80～90n/min.
24. a kind of dimeracid according to claim 17 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that water for reaction times control at 20～60min.
25. a kind of dimeracid according to claim 17 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that water for reaction times control at 30～40min.
26. a kind of dimeracid according to claim 17 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that water for temperature of reaction control at 145～155 ℃.
27. a kind of dimeracid according to claim 17 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that water for temperature of reaction control at 148～152 ℃.
28. a kind of dimeracid according to claim 1 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that the standing sedimentation dregs of fat described in the step 5 separate:
Adopt radio frequency admittance water-oil interface instrument control water-oil interface, adopt integration variable valve control input, the balance of output;
The control of standing sedimentation dregs of fat separation temperature is at 70～100 ℃;
The control of standing sedimentation dregs of fat disengaging time is at 10～60min.
29. a kind of dimeracid according to claim 28 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that the control of standing sedimentation dregs of fat separation temperature is at 80～95 ℃.
30. a kind of dimeracid according to claim 28 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that the control of standing sedimentation dregs of fat separation temperature is at 85～90 ℃.
31. a kind of dimeracid according to claim 28 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that the control of standing sedimentation dregs of fat disengaging time is at 20～50min.
32. a kind of dimeracid according to claim 28 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that the control of standing sedimentation dregs of fat disengaging time is at 30～35min.
33. a kind of dimeracid according to claim 1 filters the carclazyte pulp water and reclaims the method for thick diacid for method, it is characterized in that the slag slurry centrifuge dehydration described in the step 6:
The slag slurry is by horizontal sedimentation helical-conveyer centrifugal solid-liquid separation, and liquid enters process water pond, Gu slag enters the comprehensive utilization manufacturing procedure;
The water liquid of slag slurry centrifuge dehydration is made the process water of slurry as clay dregs hot water.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010542685 CN102010319B (en) | 2010-11-15 | 2010-11-15 | Method for reclaiming coarse diacid by using dimer acid filtered argil residue water substitution method |
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|---|---|---|---|
| CN 201010542685 CN102010319B (en) | 2010-11-15 | 2010-11-15 | Method for reclaiming coarse diacid by using dimer acid filtered argil residue water substitution method |
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| CN104529749B (en) * | 2014-12-29 | 2016-10-26 | 江苏金马油脂科技发展有限公司 | A kind of device and method reclaiming dimer (fatty acid) yl from discarded hargil |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101760326A (en) * | 2010-01-06 | 2010-06-30 | 江苏永林油脂化工有限公司 | Method for recovering fatty acid from clay dregs for dimeric dibasic acid synthesis |
| CN101843280A (en) * | 2009-11-20 | 2010-09-29 | 冀中能源邢台矿业集团有限责任公司油脂分公司 | Ground sesame seed oil fine filtering method |
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2010
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101843280A (en) * | 2009-11-20 | 2010-09-29 | 冀中能源邢台矿业集团有限责任公司油脂分公司 | Ground sesame seed oil fine filtering method |
| CN101760326A (en) * | 2010-01-06 | 2010-06-30 | 江苏永林油脂化工有限公司 | Method for recovering fatty acid from clay dregs for dimeric dibasic acid synthesis |
Non-Patent Citations (1)
| Title |
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| 李勤忠 等,.介绍几种香油生产设备.《《轻工机械》》.1991,(第03期),41-44. * |
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Address after: 224000 Nanhua Industrial Park, Jianhu County, Yancheng City, Jiangsu Province Patentee after: Jiangsu Yonglin Oil Technology Co., Ltd Address before: Nanhua Industrial Park 224700 Yancheng City Jianhu County in Jiangsu province Zhong Zhuang Patentee before: JIANGSU YONGLIN CHEMICAL OIL Co.,Ltd. |
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