CN1986508A - Tert-amyl alcohol sodium preparing process and molten sodium dispersant - Google Patents
Tert-amyl alcohol sodium preparing process and molten sodium dispersant Download PDFInfo
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- CN1986508A CN1986508A CN 200610116985 CN200610116985A CN1986508A CN 1986508 A CN1986508 A CN 1986508A CN 200610116985 CN200610116985 CN 200610116985 CN 200610116985 A CN200610116985 A CN 200610116985A CN 1986508 A CN1986508 A CN 1986508A
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- uncle
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Abstract
The present invention relates to tert-amyl alcohol sodium preparing process and molten sodium dispersant. During preparing tert-amyl alcohol sodium with sodium and tert-amyl alcohol as material, the metal salt with the general expression of MiAj is used as the dispersant, where, M represents 1-4 valent metal ion, A is acid radical, i is integral of 1-4 and j is integral of 1-3. The molten sodium dispersant of the present invention is calcium chloride, sodium chloride, titanium chloride, aluminum chloride, etc. and has sodium adsorbed onto its surface to increase the reaction surface area of sodium and speed the reaction of sodium and tert-amyl alcohol, with the reaction period being shortened to less than 12 hr.
Description
Technical field
The invention belongs to organic chemistry filed, particularly relate to and a kind ofly defend pure prepared in reaction uncle as dispersion agent by sodium and uncle with metal-salt and defend the sodium alkoxide method.
Background technology
Uncle defends sodium alkoxide and extensively is used in preparation pyrrolopyrrole diketone serial pigment as a kind of alkoxide of medium tenacity, and as United States Patent (USP) 4,579,949 is described.
Uncle defends sodium alkoxide and normally defends alcohol by sodium Metal 99.5 and uncle and defend uncle and carry out under the alcohol reflux temperature.Under this temperature, sodium fusion melts balling-up, because its surface tension is very big, is difficult for being dispersed in uncle and defends in the alcohol, so limited fully contacting of alcohol and sodium; Uncle defends the alcohol that alcohol is a higly branched chain on the other hand, and the acidity of hydroxyl is much more weak than straight chain alcohol, thereby it is very slow to make uncle defend the formation of sodium alkoxide.This is a liquid-liquid out-phase reaction, and mass transfer is the principal element of a control speed.Because sodium and uncle defend the uncompatibility of alcohol, the time of sodium complete reaction (it generally is excessive that uncle defends alcohol, calculates so the reaction times dissolves fully with sodium) needs 12-24 hour usually.For the out-phase reaction, adding fast response with phase-transfer catalyst is a very effective method.But phase-transfer catalyst obviously is unwell to sodium and uncle defends the alcohol reaction.In order to add fast response, United States Patent (USP) 4,579,949 mention with permeate agent such as sulfosuccinate di-isooctyl list sodium salt or sodium laurylsulfonate.The effect of permeate agent obviously is the surface tension that reduces Liquid Sodium, and the increase uncle defends alcohol and is in contact with it chance.
Summary of the invention
Technical problem to be solved
Technical problem to be solved by this invention provides a kind of uncle and defends the preparation method of sodium alkoxide and the dispersion agent of molten sodium, easily participate in reacting and produce unnecessary by product to overcome original permeate agent, and after the uncle who generates defends sodium alkoxide and benzene carbonitrile derivatives reaction generation pigment, be not easy to be improved speed of response greatly by the defective of flush away.
Technical scheme
One of technical scheme of the present invention provides the preparation method that a kind of uncle defends sodium alkoxide, and defending alcohol with sodium and uncle is that the feedstock production uncle defends sodium alkoxide, it is characterized in that, the metal-salt that apparatus has a following general formula is as dispersion agent:
M
iA
j
Wherein, M represents the metal ion of 1-4 valency; A represents acid group; I is the integer of 1-4; J is the integer of 1-3.
One of the optimal technical scheme that above-mentioned uncle defends the preparation method of sodium alkoxide is that said metal ions M is Li, Na, K, Ca, Ba, Sr, Mg, Sn, Al, Zn, Fe, Cu, Ni, Pb or Ti.
Above-mentioned uncle defend sodium alkoxide the preparation method optimal technical scheme two be that said acid group A is Cl
-, PO
4 -3, SO
4 -2, COO
-, CH
3COO
-, CO
3 -2Or NO
3 -
Above-mentioned uncle defend sodium alkoxide the preparation method optimal technical scheme three be that said metal-salt is an aluminum chloride.
Above-mentioned uncle defend sodium alkoxide the preparation method optimal technical scheme four be that said metal-salt is a titanium tetrachloride.
Above-mentioned uncle defend sodium alkoxide the preparation method optimal technical scheme five be that the weight ratio of said metal-salt and sodium is 0.01 to 10.
Two of technical scheme of the present invention provides a kind of dispersion agent of molten sodium, for having the metal-salt of following general formula:
M
iA
j
Wherein, M represents the metal ion of 1-4 valency; A represents acid group; I is the integer of 1-4; J is the integer of 1-3.
A kind of preferred version of the dispersion agent of above-mentioned molten sodium is that said metal-salt is an aluminum chloride.
The another kind of preferred version of the dispersion agent of above-mentioned molten sodium is that said metal-salt is a titanium tetrachloride.
Furthermore, the present invention realizes in the following manner: metal-salt is after adding reaction system, and its surface-area has a significant impact speed of reaction, so must be ground before salt is added.In employed metal-salt, find that aluminum chloride is extremely effective.Consumption about 2% (is benchmark with the sodium consumption) just can shorten to 5 hours to the reaction times.
Titanium tetrachloride adds reaction system with liquid form.It defends the little drop of emulsified formation in the alcohol uncle, this slightly drop be easy to divide beading with melting sodium, thereby increased the reaction contact area that sodium and uncle defend alcohol.So titanium tetrachloride is the most effective inorganic salt in this reaction, sodium is all dissolved generate uncle and defend sodium alkoxide.
Beneficial effect
The present invention uses metal-salt to replace organic permeate agent to accelerate to form the reaction that uncle defends sodium alkoxide greatly.Many solid metal salt surface tension are big, and liquid metal sodium spreads over its surface easily, forms fine Liquid Sodium, thereby increased the contact surface that sodium and uncle defend alcohol, can accelerate the sodium dissolution rate.Secondly, the hardness of salt is bigger, and itself can increase sodium as dispersion medium dispersion molten sodium ball under stirring action and uncle defends pure contact area.In addition, salt itself does not resemble permeate agent and easily participates in reacting the unnecessary by product of generation, and after the uncle who generates defends sodium alkoxide and benzene carbonitrile derivatives reaction generation pigment, is easy to by flush away.The consumption (with sodium consumption is benchmark) of aluminum chloride about with 2% just can shorten to 5 hours to the reaction times in employed metal-salt.Another kind of metal-salt dispersion agent titanium tetrachloride adds reaction system with liquid form, sodium is all dissolved in about 3 hours 30 minutes to generate uncle to defend sodium alkoxide.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.All inorganic chemical reagents and organic solvent are available from the Shanghai chemical reagent.
Embodiment 1
5 gram sodium Metal 99.5s add that 15 gram sodium-chlor defend in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and about 12 hours sodium all dissolves and generates uncle and defends sodium alkoxide.
The comparative example 2
5 gram sodium Metal 99.5s are defended in the alcohol high degree of agitation and are warmed to 102 ℃ 150 milliliters of uncles, and about 24 hours sodium all dissolves and generates uncle and defends sodium alkoxide.
Embodiment 3
5 gram sodium Metal 99.5s add that 0.125 gram Aluminum chloride anhydrous defends in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and about 5 hours 30 minutes sodium all dissolves and generates uncle and defends sodium alkoxide.
Embodiment 4
5 gram sodium Metal 99.5s add that 15 gram calcium chloride defend in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and about 7 hours 20 minutes sodium all dissolves and generates uncle and defends sodium alkoxide.
Embodiment 5
5 gram sodium Metal 99.5s add that 0.125 gram titanium tetrachloride defends in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and about 3 hours 30 minutes sodium all dissolves and generates uncle and defends sodium alkoxide.
Embodiment 6
5 gram sodium Metal 99.5s add that 0.125 gram sodium sulfate defends in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and sodium all dissolves and generates uncle and defend sodium alkoxide in 12 hours.
Embodiment 7
5 gram sodium Metal 99.5s add that 0.125 gram sal epsom defends in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and sodium all dissolves and generates uncle and defend sodium alkoxide in 12 hours.
Embodiment 8
5 gram sodium Metal 99.5s add that 0.125 gram bariumchloride defends in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and sodium all dissolves and generates uncle and defend sodium alkoxide in 12 hours.
Embodiment 9
5 gram sodium Metal 99.5s add that 0.125 gram zinc sulfate defends in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and sodium all dissolves and generates uncle and defend sodium alkoxide in 12 hours.
Embodiment 10
5 gram sodium Metal 99.5s add that 0.125 gram tertiary sodium phosphate defends in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and sodium all dissolves and generates uncle and defend sodium alkoxide in 12 hours.
Embodiment 11
5 gram sodium Metal 99.5s add that 0.125 gram sodium acetate defends in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and sodium all dissolves and generates uncle and defend sodium alkoxide in 12 hours.
Embodiment 12
5 gram sodium Metal 99.5s add that 0.125 gram sodium formiate defends in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and sodium all dissolves and generates uncle and defend sodium alkoxide in 12 hours.
Embodiment 13
5 gram sodium Metal 99.5s add that 0.125 gram copper sulfate defends in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and sodium all dissolves and generates uncle and defend sodium alkoxide in 12 hours.
Embodiment 14
5 gram sodium Metal 99.5s add that 0.125 gram tin chloride defends in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and sodium all dissolves and generates uncle and defend sodium alkoxide in 12 hours.
Embodiment 15
5 gram sodium Metal 99.5s add that 0.125 gram ferric sulfate defends in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and sodium all dissolves and generates uncle and defend sodium alkoxide in 12 hours.
Embodiment 16
5 gram sodium Metal 99.5s add that 0.125 gram ferrous sulfate defends in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and sodium all dissolves and generates uncle and defend sodium alkoxide in 12 hours.
Embodiment 17
5 gram sodium Metal 99.5s add that 0.125 gram strontium nitrate defends in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and sodium all dissolves and generates uncle and defend sodium alkoxide in 12 hours.
Embodiment 18
5 gram sodium Metal 99.5s add that 0.125 gram lead sulfate defends in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and sodium all dissolves and generates uncle and defend sodium alkoxide in 12 hours.
Embodiment 19
5 gram sodium Metal 99.5s add that 0.125 gram Quilonum Retard defends in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and sodium all dissolves and generates uncle and defend sodium alkoxide in 12 hours.
Embodiment 20
5 gram sodium Metal 99.5s add that 0.125 gram lime carbonate defends in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and sodium all dissolves and generates uncle and defend sodium alkoxide in 12 hours.
Embodiment 21
5 gram sodium Metal 99.5s add that 0.125 gram saltpetre defends in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and sodium all dissolves and generates uncle and defend sodium alkoxide in 12 hours.
Embodiment 22
5 gram sodium Metal 99.5s add that 0.125 gram nickelous carbonate defends in the alcohol high degree of agitation and heat 102 ℃ 150 milliliters of uncles, and sodium all dissolves and generates uncle and defend sodium alkoxide in 12 hours.
Embodiment 23
Preparation Pigment red 254
5 gram sodium Metal 99.5s add that 0.125 gram Aluminum chloride anhydrous defends in the alcohol high degree of agitation and be warmed to 102 ℃ 150 milliliters of uncles, and about 5 hours 30 minutes sodium all dissolves and generates uncle and defends sodium alkoxide.Uncle defends pure sodium solution and is cooled to 80 ℃, adds 16.58 gram dehydrations again to 6-chlorophenyl nitrile.Be heated to 110 ℃ then and in 6 hours, add 12.12 gram dehydration di-isopropyl succinates again, steam Virahol simultaneously.Finish the back and continue to stir 2 hours, be cooled to 600 ℃ then and add 82.5 ml methanol again in reaction medium.Add the mixture of 11.35 milliliters of Glacial acetic acid and 7.5 ml methanol at last, pigment is slowly separated out.The pigment of separating out is 600 ℃ of filtrations, and filter cake is used 150 ml methanol and 100 milliliters of hot washes in turn.Filter cake provides 13.9 gram Pigment reds 254 (60% yield) 700 ℃ of dryings.
Claims (9)
1. a uncle defends the preparation method of sodium alkoxide, and defending alcohol with sodium and uncle is that the feedstock production uncle defends sodium alkoxide, it is characterized in that, the metal-salt that apparatus has a following general formula is as dispersion agent:
M
iA
j
Wherein, M represents the metal ion of 1-4 valency; A represents acid group; I is the integer of 1-4; J is the integer of 1-3.
2. uncle according to claim 1 defends the preparation method of sodium alkoxide, it is characterized in that, said metal ions M is Li, Na, K, Ca, Ba, Sr, Mg, Sn, Al, Zn, Fe, Cu, Ni, Pb or Ti.
3. uncle according to claim 1 defends the preparation method of sodium alkoxide, it is characterized in that, said acid group A is Cl
-, PO
4 -3, SO
4 -2, COO
-, CH
3COO
-, CO
3 -2Or NO
3 -
4. uncle according to claim 1 defends the preparation method of sodium alkoxide, it is characterized in that, said metal-salt is an aluminum chloride.
5. uncle according to claim 1 defends the preparation method of sodium alkoxide, it is characterized in that, said metal-salt is a titanium tetrachloride.
6. defend the preparation method of sodium alkoxide according to each described uncle among the claim 1-5, it is characterized in that the weight ratio of said metal-salt and sodium is 0.01 to 10.
7. the dispersion agent of a molten sodium, for having the metal-salt of following general formula:
M
iA
j
Wherein, M represents the metal ion of 1-4 valency; A represents acid group; I is the integer of 1-4; J is the integer of 1-3.
8. the dispersion agent of molten sodium according to claim 7 is characterized in that, said metal-salt is an aluminum chloride.
9. the dispersion agent of molten sodium according to claim 7 is characterized in that, said metal-salt is a titanium tetrachloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610116985 CN1986508A (en) | 2006-10-11 | 2006-10-11 | Tert-amyl alcohol sodium preparing process and molten sodium dispersant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610116985 CN1986508A (en) | 2006-10-11 | 2006-10-11 | Tert-amyl alcohol sodium preparing process and molten sodium dispersant |
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|---|---|
| CN1986508A true CN1986508A (en) | 2007-06-27 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610116985 Pending CN1986508A (en) | 2006-10-11 | 2006-10-11 | Tert-amyl alcohol sodium preparing process and molten sodium dispersant |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102001915A (en) * | 2010-10-19 | 2011-04-06 | 常州吉恩化工有限公司 | Manufacturing method of granular sodium tert-pentoxide |
| CN101565354B (en) * | 2009-06-05 | 2011-12-28 | 山东中氟化工科技有限公司 | Method for preparing fluorine-containing sodium alkyl alcohol |
-
2006
- 2006-10-11 CN CN 200610116985 patent/CN1986508A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565354B (en) * | 2009-06-05 | 2011-12-28 | 山东中氟化工科技有限公司 | Method for preparing fluorine-containing sodium alkyl alcohol |
| CN102001915A (en) * | 2010-10-19 | 2011-04-06 | 常州吉恩化工有限公司 | Manufacturing method of granular sodium tert-pentoxide |
| CN102001915B (en) * | 2010-10-19 | 2013-11-06 | 常州吉恩化工有限公司 | Manufacturing method of granular sodium tert-pentoxide |
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