CN107698475A - Synthesis process of liquid xanthate under solvent-free condition - Google Patents
Synthesis process of liquid xanthate under solvent-free condition Download PDFInfo
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- CN107698475A CN107698475A CN201710713201.XA CN201710713201A CN107698475A CN 107698475 A CN107698475 A CN 107698475A CN 201710713201 A CN201710713201 A CN 201710713201A CN 107698475 A CN107698475 A CN 107698475A
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- solution
- liquid
- butyl
- xanthate
- carbon disulfide
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C329/00—Thiocarbonic acids; Halides, esters or anhydrides thereof
- C07C329/12—Dithiocarbonic acids; Derivatives thereof
- C07C329/14—Esters of dithiocarbonic acids
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
the invention relates to the technical field of synthesis of sulfide ore collecting agents, in particular to a synthesis process of liquid xanthate under a solvent-free condition, which comprises the steps of synthesizing the liquid butyl sodium/butyl potassium xanthate under the condition of not containing an organic solvent, firstly adding butanol and carbon disulfide solution into a three-neck flask provided with a thermometer, a stirrer, a dropping funnel, a condensing tube and a water bath kettle, heating and raising the temperature to 28-35 ℃ after fully stirring the mixed solution, then slowly dropping caustic alkali solution into the mixed solution in the three-neck flask at the dropping speed of 1-3 m L/min while stirring, and preserving the temperature and fully stirring after the dropping of the caustic solution is finished to prepare the liquid butyl sodium/butyl potassium xanthate.
Description
Technical field
The present invention relates to a kind of synthesis technical field of sulfide mineral collector, liquid under specifically a kind of condition of no solvent
The synthesis technique of body xanthate.
Background technology
Butyl sodium/butyl potassium xanthate is that mine using a kind of extensive non-ferrous metal collecting agent, has choosing both at home and abroad at present
The characteristics of selecting property is good, and collecting ability is moderate, it is important application of the Organic Chemicals in mining processing industry.Xanthate is produced at present
Main method has：
（1）Solvent method：I.e. carbon disulfide and alcohol have in a large amount of benzene,toluene,xylenes, ethylbenzene, gasoline, kerosene, dichloroethanes etc.
Reacted in solvent, then add alkali effect, the xanthate of generation crystallizes out in the solution, filtered re-dry and produced
Product.The xanthate quality produced in this way is good, but introduces the higher organic solvent of boiling point, and organic solvent recycling is compared
Difficulty, cost are too high.
（2）Direct synthesis technique：The method directly acts on alcohol, caustic alkali and carbon disulfide, and biggest advantage is without other
Auxiliary material, without any solvent, production process is simple, and cost is low；Shortcoming is solid exothermic reaction, to the fully mixed of raw material
Close, the control of reaction temperature has higher requirement, if dealt with improperly, product purity can be caused not high.
The content of the invention
It is an object of the invention to provide a kind of synthesis technique of liquid xanthate under condition of no solvent, can solve institute in solvent method
The problem of organic solvent is not easily recycled processing, and the control of direct synthesis technique reaction temperature requires high, and production cost is high.
To reach above-mentioned purpose, the technical solution used in the present invention is：
The synthesis technique of liquid xanthate under a kind of condition of no solvent, present invention synthetic fluid under conditions of organic solvent is not contained
Butyl sodium/butyl potassium xanthate, it is characterised in that：It comprises the following steps：
Step 1: equipped with thermometer, agitator, dropping funel, condenser pipe, water-bath three-necked flask in, be firstly added fourth
The mol ratio of alcohol, carbon disulfide solution, butanol and carbon disulfide is 1.0~2.0:1.0~1.5；Be stirred solution 0.5~
2h, then it is heated to 28~35 DEG C；
Step 2: caustic solution is slowly dropped into the mixed solution in three-necked flask, rate of addition is controlled in 1~3mL/
Min, stirred when being added dropwise, the caustic solution and the mol ratio of carbon disulfide being added dropwise to are 1:1.0~1.5；Causticity alkali soluble
The reaction temperature of solution is controlled at 20~30 DEG C during drop adds；
Step 3: after treating step 2 completion of dropwise addition, it is incubated under the conditions of 22~28 DEG C and stirs 1~5h, liquid butyl is made
Sodium/butyl potassium xanthate, the molecular formula of liquid butyl sodium/butyl potassium xanthate of synthesis are：, wherein R
For normal-butyl or isobutyl group one kind therein, Me is sodium ion or potassium ion.
Preferably, the caustic solution uses any of sodium hydroxide solution or potassium hydroxide solution, caustic alkali
The mass percent concentration of solution is 35~40%.
Preferably, the butanol is one kind in n-butanol or isobutanol.
Preferably, the butanol, carbon disulfide, caustic solution are AR.
The present invention uses solventless method, butanol and carbon disulfide is sufficiently stirred into mixing in three-necked flask first, then
Caustic solution is slowly added to, once completes course of reaction, generation liquid butyl sodium/butyl potassium xanthate.In step 1 of the present invention,
The equation that butanol, carbon disulfide and caustic solution chemically react under these conditions is as follows：
Wherein R is respectively normal-butyl or isobutyl group one kind therein, and Me is sodium ion or potassium ion.This reaction is exothermic reaction.
The preparation method of liquid xanthate of the present invention operates at ambient pressure, by the dropwise addition speed for controlling caustic solution
Degree carrys out controlling reaction temperature, and raw material mixing, reaction are abundant.With technique is simple, yield is high, good product quality, easy to use, raw
Produce low cost and other advantages.
Embodiment
With reference to embodiment, the present invention is described in further detail, it will be appreciated that described herein excellent
Select embodiment to be merely to illustrate and explain the present invention, be not intended to limit the present invention.
Embodiment 1
A kind of liquid butyl sodium（Potassium）The synthesis technique of xanthate, it comprises the following steps：
Step 1: equipped with thermometer, agitator, dropping funel, condenser pipe, water-bath three-necked flask in, add n-butanol,
The mol ratio of carbon disulfide, n-butanol and carbon disulfide is 1.0:1.5；Solution 2h is stirred, then it is heated to 30~
35℃；
Step 2: the sodium hydroxide solution that mass percent concentration is 40% is slowly dropped into the mixed solution in three-necked flask,
Rate of addition is controlled in 3mL/min, is stirred when being added dropwise, the sodium hydroxide solution and the mol ratio of carbon disulfide being added dropwise to are
1: 1.5；The reaction temperature of solution is controlled at 25~30 DEG C during sodium hydroxide solution is added dropwise；
Step 3: after treating step 2 completion of dropwise addition, it is incubated at 28 DEG C and stirs 5h, liquid normal-butyl sodium xanthate is made.
Through check analysis, the liquid normal-butyl prepared by the present embodiment receive xanthate mass percentage content be 92.1%, instead
It is 94.3% to answer yield.
Embodiment 2
A kind of liquid butyl sodium（Potassium）The synthesis technique of xanthate, it comprises the following steps：
Step 1: equipped with thermometer, agitator, dropping funel, condenser pipe, water-bath three-necked flask in, add n-butanol,
The mol ratio of carbon disulfide, n-butanol and carbon disulfide is 2.0:1.5；Solution 2h is stirred, then it is heated to 28~
30℃；
Step 2: the potassium hydroxide solution that mass percent concentration is 35% is slowly dropped into the mixed solution in three-necked flask,
Rate of addition is controlled in 1mL/min, is stirred when being added dropwise, the potassium hydroxide solution and the mol ratio of carbon disulfide being added dropwise to are
1: 1；The reaction temperature of solution is controlled at 20~30 DEG C during potassium hydroxide solution is added dropwise；
Step 3: after treating step 2 completion of dropwise addition, it is incubated under the conditions of 22 DEG C and stirs 3h, it is yellow that liquid normal-butyl potassium is made
Medicine.
Through check analysis, the mass percentage content of the liquid normal-butyl potassium xanthate prepared by the present embodiment is 89.7%, instead
It is 90.1% to answer yield.
Embodiment 3
A kind of liquid butyl sodium（Potassium）The synthesis technique of xanthate, it comprises the following steps：
Step 1: equipped with thermometer, agitator, dropping funel, condenser pipe, water-bath three-necked flask in, add isobutanol,
The mol ratio of carbon disulfide, isobutanol and carbon disulfide is 1.5:1.0；Solution 2h is stirred, then it is heated to 30~
32℃；
Step 2: the sodium hydroxide solution that mass percent concentration is 35% is slowly dropped into the mixed solution in three-necked flask,
Rate of addition is controlled in 2.5mL/min, is stirred when being added dropwise, the sodium hydroxide solution and the mol ratio of carbon disulfide being added dropwise to
For 1: 1.2；The reaction temperature of solution is controlled at 25~30 DEG C during sodium hydroxide solution is added dropwise；
Step 3: after treating step 2 completion of dropwise addition, it is incubated under the conditions of 25 DEG C and stirs 3h, it is yellow that liquid isobutyl group sodium is made
Medicine.
Through check analysis, the mass percentage content of the liquid isobutyl group sodium xanthate prepared by the present embodiment is 88.3%, instead
It is 90.5% to answer yield.
Embodiment 4
A kind of liquid butyl sodium（Potassium）The synthesis technique of xanthate, it comprises the following steps：
Step 1: equipped with thermometer, agitator, dropping funel, condenser pipe, water-bath three-necked flask in, add isobutanol,
The mol ratio of carbon disulfide, isobutanol and carbon disulfide is 2.0:1.0；Solution 1.5h is stirred, is then heated to 32
℃；
Step 2: the potassium hydroxide solution that mass percent concentration is 38% is slowly dropped into the mixed solution in three-necked flask,
Rate of addition is controlled in 2mL/min, is stirred when being added dropwise, the potassium hydroxide solution and the mol ratio of carbon disulfide being added dropwise to are
1: 1.2；The reaction temperature of solution is controlled at 20~30 DEG C during caustic solution is added dropwise；
Step 3: after treating step 2 completion of dropwise addition, it is incubated under the conditions of 28 DEG C and stirs 4h, it is yellow that liquid isobutyl group potassium is made
Medicine.
Through check analysis, the mass percentage content of the liquid isobutyl group potassium xanthate prepared by the present embodiment is 87.6%, instead
It is 91.1% to answer yield.
In the above-described embodiments, the butanol, carbon disulfide, caustic solution are AR.
The present invention needs strictly to control the process conditions such as the raw material proportioning in each step, reaction temperature, time difference occur
Side reaction is had, such as：Carbon disulfide and caustic solution effect, generation sulfide, thiocarbonate and carbonate etc., this
A little side reactions can all influence product quality.
Claims (4)
1. the synthesis technique of liquid xanthate under a kind of condition of no solvent, present invention Synthesis liquid under conditions of organic solvent is not contained
Body butyl sodium/butyl potassium xanthate, it is characterised in that：It comprises the following steps：
Step 1: equipped with thermometer, agitator, dropping funel, condenser pipe, water-bath three-necked flask in, be firstly added fourth
The mol ratio of alcohol, carbon disulfide solution, butanol and carbon disulfide is 1.0~2.0:1.0~1.5；Be stirred solution 0.5~
2h, then it is heated to 28~35 DEG C；
Step 2: caustic solution is slowly dropped into the mixed solution in three-necked flask, rate of addition is controlled in 1~3mL/
Min, stirred when being added dropwise, the caustic solution and the mol ratio of carbon disulfide being added dropwise to are 1:1.0~1.5；Causticity alkali soluble
The reaction temperature of solution is controlled at 20~30 DEG C during drop adds；
Step 3: after treating step 2 completion of dropwise addition, it is incubated under the conditions of 22~28 DEG C and stirs 1~5h, liquid butyl is made
Sodium/butyl potassium xanthate, the molecular formula of liquid butyl sodium/butyl potassium xanthate of synthesis are：, wherein R
For normal-butyl or isobutyl group one kind therein, Me is sodium ion or potassium ion.
2. the synthesis technique of liquid xanthate under a kind of condition of no solvent according to claim 1, it is characterised in that：It is described severe
Property aqueous slkali uses any of sodium hydroxide solution or potassium hydroxide solution, and the mass percent concentration of caustic solution is
35~40%.
3. the synthesis technique of liquid xanthate under a kind of condition of no solvent according to claim 1, it is characterised in that：The fourth
Alcohol is one kind in n-butanol or isobutanol.
4. the synthesis technique of liquid xanthate under a kind of condition of no solvent according to claim 1 or 2, it is characterised in that：Institute
It is AR to state butanol, carbon disulfide, caustic solution.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710713201.XA CN107698475A (en) | 2017-08-18 | 2017-08-18 | Synthesis process of liquid xanthate under solvent-free condition |
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| CN201710713201.XA CN107698475A (en) | 2017-08-18 | 2017-08-18 | Synthesis process of liquid xanthate under solvent-free condition |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3767692A (en) * | 1971-05-31 | 1973-10-23 | Canadian Ind | Xanthate manufacture |
| CN102050769A (en) * | 2009-11-11 | 2011-05-11 | 黄军 | Process for synthesizing sodium butyl xanthate |
-
2017
- 2017-08-18 CN CN201710713201.XA patent/CN107698475A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3767692A (en) * | 1971-05-31 | 1973-10-23 | Canadian Ind | Xanthate manufacture |
| CN102050769A (en) * | 2009-11-11 | 2011-05-11 | 黄军 | Process for synthesizing sodium butyl xanthate |
Non-Patent Citations (5)
| Title |
|---|
| 仵亚妮 等: "液体黄药生产工艺的改进及其选矿实验，仵亚妮 等，化工生产与技术，第21卷第4期，第17-18，47页", 《化工生产与技术》 * |
| 冶金工业部有色金属研究院 著: "《浮选机制造法 第1辑》", 29 February 1960, 冶金工业出版社 * |
| 施先义 等: "丁基钠黄药合成工艺的改进", 《化工技术与开发》 * |
| 杨晓玲 等: "液体异丙基黄原酸钠的合成", 《应用化工》 * |
| 胡正吉 等: "溶剂法生产异丁基钾黄药", 《有色矿冶》 * |
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Application publication date: 20180216 |