CN103864568A - Process and equipment for preparing chloropentane - Google Patents
Process and equipment for preparing chloropentane Download PDFInfo
- Publication number
- CN103864568A CN103864568A CN201410091127.9A CN201410091127A CN103864568A CN 103864568 A CN103864568 A CN 103864568A CN 201410091127 A CN201410091127 A CN 201410091127A CN 103864568 A CN103864568 A CN 103864568A
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- CN
- China
- Prior art keywords
- isopentene
- reaction
- hydrogen chloride
- phosphorus trichloride
- chloride gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000000034 method Methods 0.000 title claims abstract description 19
- SQCZQTSHSZLZIQ-UHFFFAOYSA-N 1-chloropentane Chemical compound CCCCCCl SQCZQTSHSZLZIQ-UHFFFAOYSA-N 0.000 title abstract 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 79
- 239000007789 gas Substances 0.000 claims abstract description 46
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 38
- YHQXBTXEYZIYOV-UHFFFAOYSA-N 3-methylbut-1-ene Chemical compound CC(C)C=C YHQXBTXEYZIYOV-UHFFFAOYSA-N 0.000 claims abstract description 28
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 238000010521 absorption reaction Methods 0.000 claims abstract description 12
- 230000035484 reaction time Effects 0.000 claims abstract description 9
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 8
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 5
- 230000007062 hydrolysis Effects 0.000 claims abstract description 4
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 60
- 239000011552 falling film Substances 0.000 claims description 34
- 238000002360 preparation method Methods 0.000 claims description 25
- 238000005516 engineering process Methods 0.000 claims description 17
- 239000007921 spray Substances 0.000 claims description 9
- 238000007259 addition reaction Methods 0.000 claims description 7
- BKOOMYPCSUNDGP-UHFFFAOYSA-N 2-methylbut-2-ene Chemical group CC=C(C)C BKOOMYPCSUNDGP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000945 filler Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- -1 (2) Chemical compound 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 abstract description 6
- 239000006227 byproduct Substances 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 6
- 238000011084 recovery Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000006353 environmental stress Effects 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- PJGSXYOJTGTZAV-UHFFFAOYSA-N pinacolone Chemical compound CC(=O)C(C)(C)C PJGSXYOJTGTZAV-UHFFFAOYSA-N 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a process for preparing chloropentane. The process comprises the steps: hydrolyzing phosphorus trichloride, performing isopentene addition and recovering hydrogen chloride gas. The process is characterized in that the process of hydrolyzing phosphorus trichloride comprises the substeps: adding diluted hydrochloric acid with the mass percentage of 3-5 percent and phosphorus trichloride into a reaction kettle for reacting, wherein the reaction temperature is 30-50 DEG C, and the reaction time is 4 hours; the process of performing isopentene addition comprises the substeps: contacting isopentene and hydrogen chloride gas for reacting, wherein the gas flow velocity is 150m<3>/h, the reaction temperature is 5-10 DEG C, and the reaction time is 20-30 seconds; and absorbing excessive hydrogen chloride gas through a hydrochloric acid absorption tower to be used for hydrolyzing phosphorus trichloride again. The process has the beneficial effects that the phosphorus trichloride hydrolysis condition is adjusted to the temperature of 30-50 DEG C and the reaction time of 4 hours, the problems that heat release is extremely fast and the gas release amount is instable in the reaction process are effectively solved, the potential safety hazard is eliminated, a good reaction basis is provided for subsequent addition, the content of by-product phosphorous acid is over 99 percent, the yield is improved to over 99 percent, and the economic benefits are considerable.
Description
Technical field
The preparation technology and the equipment that the present invention relates to a kind of chlorinated special pentane, belong to chemical technology field.
Background technology
Pinacolone, mainly for the production of triazole pesticide, also for the production of weedicide and pharmaceutical prod, is one of important industrial chemicals.In the preparation technology of pinacolone, chlorinated special pentane is again very important intermediate.
In the existing technique of preparing chlorinated special pentane, conventionally adopt hydrochloric acid additive process, that is: quantitative isopentene under 5 ± 2 DEG C of conditions with excessive hydrochloric acid reaction, hydrochloric acid time for adding, at 2.5-3h, also needs to be incubated 2h after being added dropwise to complete conventionally.Because the add-on of this technique hydrochloric acid is too large, produce a large amount of spent acid and cause aftertreatment more difficult, and production efficiency is not high, impurity is more, product relative content is lower, so need to transform the technology of preparing of chlorinated special pentane.At application number be: in 201210009392.9 Chinese patent, by coproduction phosphorous acid, use byproduct hydrogen chloride gas and the isopentene of phosphorous acid to carry out addition, thereby reduced the add-on of hydrochloric acid and the quantity discharged of waste water, the relative content of production efficiency and product also increases.But in actual production, the process heat release of phosphorus trichloride hydrolysis generation phosphorous acid is too fast, hydrogen chloride gas burst size is unstable, not only there is certain potential safety hazard, and the addition reaction meeting of follow-up hydrogen chloride gas and isopentene is produced to certain impact, thereby affected content and the productive rate of chlorinated special pentane, so also need above-mentioned technique to improve.
Summary of the invention
For solving the deficiencies in the prior art, thereby the object of the present invention is to provide a kind of evenly heat release, Stable Release hydrogen chloride gas to ensure the preparation technology of the chlorinated special pentane that reacting balance carries out and the equipment using in preparation process.
In order to realize above-mentioned target, the present invention adopts following technical scheme:
A kind of preparation technology of chlorinated special pentane, comprise the following steps: the hydrolysis of (), phosphorus trichloride, (2), isopentene addition, (3), hydrogen chloride gas reclaims, it is characterized in that, the hydrolytic process of phosphorus trichloride is: the dilute hydrochloric acid and the phosphorus trichloride that are 3-5% by quality percentage composition are put into reaction kettle for reaction, and temperature of reaction is 30-50 DEG C, and the reaction times is 4h; Isopentene addition process is: isopentene is contacted and reacted with hydrogen chloride gas, and gas flow rate is 150m
3/ h, temperature of reaction is 5-10 DEG C, the reaction times is 20-30s; Hydrogen chloride gas excessive after isopentene addition is again hydrolyzed for phosphorus trichloride after hydrochloric acid absorption tower absorbs.
The preparation technology of aforesaid chlorinated special pentane, is characterized in that, it is 300-320kg/h that phosphorus trichloride adds the speed of reactor.
The preparation technology of aforesaid chlorinated special pentane, is characterized in that, the addition reaction of isopentene and hydrogen chloride gas is carried out in falling-film tower, and isopentene sprays downwards from tower top, and hydrogen chloride gas is from introducing with micro-vacuum at the bottom of tower.
The preparation technology of aforesaid chlorinated special pentane, is characterized in that, the flow velocity of isopentene is 680L/h, and temperature is 3-7 DEG C.
The preparation technology of aforesaid chlorinated special pentane, is characterized in that, the temperature of falling-film tower bottom is 8-12 DEG C.
A kind of equipment for the preparation of chlorinated special pentane, comprise: reactor, the falling-film tower being connected with reactor, the hydrochloric acid absorption tower being connected with falling-film tower, it is characterized in that, also comprise: the self-feeding bucket being connected with reactor, is provided with under meter on aforementioned self-feeding bucket.
The aforesaid equipment for the preparation of chlorinated special pentane, is characterized in that, on the isoamylene feed pipeline of falling-film tower, be provided with volume pump on hydrogen chloride gas feed pipe.
The aforesaid equipment for the preparation of chlorinated special pentane, is characterized in that, the bottom of falling-film tower is provided with the first thermometer, and the position contour with spray header is provided with the second thermometer.
The aforesaid equipment for the preparation of chlorinated special pentane, is characterized in that, the inside of falling-film tower is provided with filler.
Usefulness of the present invention is: the hydrolysising condition of phosphorus trichloride is adjusted into 30-50 DEG C, reaction 4h, efficiently solve that reaction process heat release is too fast, the unsettled problem of air release amount, not only eliminate potential safety hazard, and provide the good basis of reacting for follow-up hydrogen chloride gas and the addition of isopentene, and the content of byproduct phosphorous acid reaches more than 99%, yield also brings up to 99%, economic benefits; The addition process of hydrogen chloride gas and isopentene adopts falling-film tower spraying technique, and spray, without dead angle, efficiently solves reactant and contacts inadequate problem; Excessive hydrogen chloride gas also can continue on for, in the hydrolysis reaction of phosphorus trichloride, having accomplished to recycle completely after hydrochloric acid absorption tower absorbs, and neither waste, has alleviated again environmental stress.
Brief description of the drawings
Fig. 1 is the composition schematic diagram of the equipment for the preparation of chlorinated special pentane of the present invention.
The implication of Reference numeral in figure: 1-reactor, 2-falling-film tower, 3-hydrochloric acid absorption tower, 4-self-feeding bucket, 5-under meter, 6-volume pump, 7-the first thermometer, 8-the second thermometer, 9-spray header, 10-hydrogen chloride gas recovery channel, 11-hydrogenchloride liquids recovery pipeline, arrow represents the flow direction of hydrogenchloride.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is done to concrete introduction.
Paper is prepared chlorinated special pentane equipment used.
With reference to Fig. 1, the equipment for the preparation of chlorinated special pentane of the present invention comprises: reactor 1, the falling-film tower 2 being connected with reactor 1 and self-feeding bucket 4 and the hydrochloric acid absorption tower 3 being connected with falling-film tower 2.
Concrete, self-feeding bucket 4 is connected with the top of reactor 1, for automatically adding reactant to reactor 1, is provided with the under meter 5 for metered reagent flow on it; The top of reactor 1 is provided with gas output tube road, and this gas output tube road is communicated with the hydrogen chloride gas feed pipe of falling-film tower 2, and hydrogen chloride gas feed pipe is arranged on the bottom of falling-film tower 2, and the top of falling-film tower 2 is provided with isoamylene feed pipeline; The top of falling-film tower 2 is also provided with hydrogen chloride gas recovery channel 10, and this pipeline is communicated with hydrochloric acid absorption tower 3; The bottom of hydrochloric acid absorption tower 3 is provided with hydrogenchloride liquids recovery pipeline 11, and this pipeline is communicated with hydrochloric acid self-feeding bucket 4, thereby has realized the recycle of hydrochloric acid, has both effectively alleviated environmental stress, and the cost of saving again drops into, economic benefits.
As the preferred scheme of one, on the isoamylene feed pipeline of falling-film tower 2, be provided with volume pump 6 on hydrogen chloride gas feed pipe.
More preferably, the bottom of falling-film tower 2 is provided with the first thermometer 7, for monitoring the temperature of falling-film tower 2 bottoms; The position contour with spray header 9 is provided with the second thermometer 8, the temperature when monitoring liquid, gas contact reacts.
In order to ensure that the interior liquid of falling-film tower 2, gas mix and contact completely, as the preferred scheme of one, the inside of falling-film tower 2 is provided with filler (not shown), and the height of filler is preferably 0.8 times of falling-film tower 2 height.
It should be noted that, temperature control system adopts the setting of this area routine, not shown, does not also repeat.
Introduce and utilize aforesaid device to prepare the process of chlorinated special pentane below.
First the dilute hydrochloric acid that is, 3-5% by quality percentage amounts joins in reactor 1 by self-feeding bucket 4; Then, by another self-feeding bucket 4, phosphorus trichloride is joined in reactor 1, the speed adding is 300-320kg/h; Next, make dilute hydrochloric acid be hydrolyzed and react in reactor 1 with phosphorus trichloride, temperature of reaction is 30-50 DEG C, and the reaction times is 4h; The hydrogen chloride gas generating in reactor 1, via gas output tube road, hydrogen chloride gas feed pipe, is incorporated in falling-film tower 2 with micro-vacuum, and gas flow rate is 150m
3/ h; Isopentene sprays downwards from falling-film tower 2 tower tops via spray header 9 by isoamylene feed pipeline, and the flow velocity of isopentene is 680L/h, enters falling-film tower 2 and is first cooled to 3-7 DEG C before; The catalytic time of isopentene and hydrogen chloride gas is 20-30s, and temperature of reaction is 5-10 DEG C, and in whole process, the temperature of falling-film tower 2 bottoms is controlled at 8-12 DEG C; Hydrogen chloride gas excessive in falling-film tower 2 enters into hydrochloric acid absorption tower 3 through hydrogen chloride gas recovery channel 10, after absorption, obtain dilute hydrochloric acid, in the time that the quality percentage composition of dilute hydrochloric acid reaches 3-5%, enter into dilute hydrochloric acid self-feeding bucket 4, utilization to be recycled via hydrogenchloride liquids recovery pipeline 11 again.
Above-mentioned falling-film tower tower height 10m, diameter 0.6m, the inner high 8m of filler.
The impact of embodiment 1-3 temperature on phosphorus trichloride hydrolysis reaction, in table 1:
The impact of table 1 temperature on phosphorus trichloride hydrolysis reaction
In the various embodiments described above, through observing, hydrolysis reaction heat release is comparatively even, and the burst size of the hydrogen chloride gas generating is also comparatively steady, and as shown in Table 1, the content of by product phosphorous acid and yield have all reached more than 99%, economic benefits.
The impact of embodiment 4-10 temperature on isopentene addition reaction
Product chlorinated special pentane in embodiment 4-10 is carried out to assay, employing be the gas chromatograph with hydrogen flame, the concrete parameter of setting is:
Chromatographic column: 30m × 0.3mm, thickness 0.45 μ m, 0V-01 capillary column, sensitivity (yang)=1, splitting ratio 1:100, carrier gas is nitrogen, 180 DEG C of sensing chamber's temperature, 180 DEG C of temperature of vaporization chamber, 50 DEG C of column temperature starting temperatures, keep 2min, are warmed up to 100 DEG C with 10 DEG C/min.
Temperature on the impact of isopentene addition reaction referring to table 2.
The impact of table 2 temperature on isopentene addition reaction
Can be found out by upper watch test data, when isoamylene feed temperature is at 3-7 DEG C, flow velocity 680L/h, hydrogen chloride gas rate of flow of fluid 150m
3/ h, gas, liquid contact reacts temperature are at 5-10 DEG C, reaction times during at 20-30s, and the product content that addition reaction obtains has been brought up to more than 97.5%, and product output has been brought up to more than 92.0%.
It should be noted that, above-described embodiment does not limit the present invention in any form, and all employings are equal to replaces or technical scheme that the mode of equivalent transformation obtains, all drops in protection scope of the present invention.
Claims (9)
1. the preparation technology of chlorinated special pentane, comprise the following steps: the hydrolysis of (), phosphorus trichloride, (2), isopentene addition, (3), hydrogen chloride gas reclaims, it is characterized in that, the hydrolytic process of phosphorus trichloride is: the dilute hydrochloric acid and the phosphorus trichloride that are 3-5% by quality percentage composition are put into reaction kettle for reaction, and temperature of reaction is 30-50 DEG C, and the reaction times is 4h; Isopentene addition process is: isopentene is contacted and reacted with hydrogen chloride gas, and gas flow rate is 150m
3/ h, temperature of reaction is 5-10 DEG C, the reaction times is 20-30s; Hydrogen chloride gas excessive after isopentene addition is again hydrolyzed for phosphorus trichloride after hydrochloric acid absorption tower absorbs.
2. the preparation technology of chlorinated special pentane according to claim 1, is characterized in that, it is 300-320kg/h that phosphorus trichloride adds the speed of reactor.
3. the preparation technology of chlorinated special pentane according to claim 1, is characterized in that, the addition reaction of isopentene and hydrogen chloride gas is carried out in falling-film tower, and isopentene sprays downwards from tower top, and hydrogen chloride gas is from introducing with micro-vacuum at the bottom of tower.
4. the preparation technology of chlorinated special pentane according to claim 3, is characterized in that, the flow velocity of isopentene is 680L/h, and temperature is 3-7 DEG C.
5. the preparation technology of chlorinated special pentane according to claim 4, is characterized in that, the temperature of falling-film tower bottom is 8-12 DEG C.
6. the equipment for the preparation of chlorinated special pentane, comprise: reactor, the falling-film tower being connected with reactor, the hydrochloric acid absorption tower being connected with falling-film tower, it is characterized in that, also comprise: the self-feeding bucket being connected with reactor, is provided with under meter on described self-feeding bucket.
7. the equipment for the preparation of chlorinated special pentane according to claim 6, is characterized in that, on the isoamylene feed pipeline of falling-film tower, be provided with volume pump on hydrogen chloride gas feed pipe.
8. the equipment for the preparation of chlorinated special pentane according to claim 7, is characterized in that, the bottom of falling-film tower is provided with the first thermometer, and the position contour with spray header is provided with the second thermometer.
9. according to the equipment for the preparation of chlorinated special pentane described in claim 6-8 any one, it is characterized in that, the inside of falling-film tower is provided with filler.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410091127.9A CN103864568A (en) | 2014-03-13 | 2014-03-13 | Process and equipment for preparing chloropentane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410091127.9A CN103864568A (en) | 2014-03-13 | 2014-03-13 | Process and equipment for preparing chloropentane |
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| Publication Number | Publication Date |
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| CN103864568A true CN103864568A (en) | 2014-06-18 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410091127.9A Pending CN103864568A (en) | 2014-03-13 | 2014-03-13 | Process and equipment for preparing chloropentane |
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| CN (1) | CN103864568A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104961634A (en) * | 2015-05-25 | 2015-10-07 | 张家港市振方化工有限公司 | Method for preparing high yield pinacolone, and pesticide bactericide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101823704A (en) * | 2009-03-06 | 2010-09-08 | 南通江山农药化工股份有限公司 | Method for continuously synthesizing phosphorous acid |
| CN102249202A (en) * | 2011-06-16 | 2011-11-23 | 江苏大明科技有限公司 | Preparation process for synthesizing phosphorous acid by hydrolyzing phosphorous trichloride |
| CN102295517A (en) * | 2011-07-05 | 2011-12-28 | 镇江市东煌化工有限公司 | Process of synthesizing methyl chloride with hydrogen chloride gas by-produced in production of phosphorous acid from phosphorus trichloride |
| CN102557860A (en) * | 2012-01-13 | 2012-07-11 | 张家港市振方化工有限公司 | Preparation method of chlorinated special pentane |
| CN103350990A (en) * | 2013-08-06 | 2013-10-16 | 河南清水源科技股份有限公司 | Process for preparing phosphorous acid by hydrolyzing phosphorus trichloride |
| CN203728742U (en) * | 2014-03-13 | 2014-07-23 | 张家港市振方化工有限公司 | Equipment for preparing chloropivaloyl pentane |
-
2014
- 2014-03-13 CN CN201410091127.9A patent/CN103864568A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101823704A (en) * | 2009-03-06 | 2010-09-08 | 南通江山农药化工股份有限公司 | Method for continuously synthesizing phosphorous acid |
| CN102249202A (en) * | 2011-06-16 | 2011-11-23 | 江苏大明科技有限公司 | Preparation process for synthesizing phosphorous acid by hydrolyzing phosphorous trichloride |
| CN102295517A (en) * | 2011-07-05 | 2011-12-28 | 镇江市东煌化工有限公司 | Process of synthesizing methyl chloride with hydrogen chloride gas by-produced in production of phosphorous acid from phosphorus trichloride |
| CN102557860A (en) * | 2012-01-13 | 2012-07-11 | 张家港市振方化工有限公司 | Preparation method of chlorinated special pentane |
| CN103350990A (en) * | 2013-08-06 | 2013-10-16 | 河南清水源科技股份有限公司 | Process for preparing phosphorous acid by hydrolyzing phosphorus trichloride |
| CN203728742U (en) * | 2014-03-13 | 2014-07-23 | 张家港市振方化工有限公司 | Equipment for preparing chloropivaloyl pentane |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104961634A (en) * | 2015-05-25 | 2015-10-07 | 张家港市振方化工有限公司 | Method for preparing high yield pinacolone, and pesticide bactericide |
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Application publication date: 20140618 |