CN106542967A - A kind of solid sodium methylate preparation method - Google Patents
A kind of solid sodium methylate preparation method Download PDFInfo
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- CN106542967A CN106542967A CN201610943451.8A CN201610943451A CN106542967A CN 106542967 A CN106542967 A CN 106542967A CN 201610943451 A CN201610943451 A CN 201610943451A CN 106542967 A CN106542967 A CN 106542967A
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- China
- Prior art keywords
- sodium methylate
- solid sodium
- mixture
- toluene
- methanol
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/86—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a kind of solid sodium methylate preparation method, and the method includes：Liquid methanol sodium is mixed homogeneously with toluene, mixture a is formed；Mixture a is warming up to into 95 105 DEG C under vacuum, 10 15h is stirred, is obtained mixture b and methanol；Mixture b is warming up to into 130 150 DEG C under vacuum, 6 8h is stirred, is obtained solid sodium methylate and toluene.Addition of the solid sodium methylate preparation method that the present invention is provided by toluene so that methanol from liquid methanol sodium can be detached and is dissolved completely in toluene solution, and then realize that the gradation of methanol and toluene is steamed by step heating.When the solid sodium methylate preparation method that the present invention is provided can not only solve the problems, such as that liquid methanol sodium is dried in existing process, viscosity is big, solid sodium methylate caking, and prepared solid sodium methylate has the characteristics of total alkali is high, purity is high, free alkali is low, product specific volume is little and active high, it is adaptable to promote on a large scale and application.
Description
Technical field
The present invention relates to Feldalat NM preparing technical field, more particularly to a kind of solid sodium methylate preparation method.
Background technology
Solid sodium methylate is a kind of white-amorphous free-flowing powder, odorless, and be soluble in ethanol and methanol.Solid methanol
Sodium is more sensitive to air and dampness, resolves into rapidly methanol and sodium hydroxide when water is met.Solid sodium methylate is not only to air
It is more sensitive with dampness, and easily decompose in the air under the conditions of 126 DEG C, property is unstable.
Solid sodium methylate is usually to be prepared from through drying by liquid methanol sodium in the preparation.As liquid methanol sodium is
The mixture of Feldalat NM and methanol, with the carrying out of liquid methanol sodium dry run, liquid methanol sodium is more and more sticky, last shape
Into dope, methanol can not be completely disengaged from from liquid methanol sodium.The drying of liquid methanol sodium is the drying of dope, is contained
There is the solid sodium methylate of the bulk solid shape of residual methanol, and prepared solid sodium methylate total alkali is low, purity is low, free alkali
Height, product specific volume is big, activity is low.When the solid sodium methylate of solid, shaped is prepared into pulverulent solids Feldalat NM, it usually needs use
Stamp taps into powder, then so that there is the big defect of airborne dust in the production process of solid sodium methylate.Further, since solid
Feldalat NM easily makes moist, spontaneous combustion and with strong corrosivity, thus the solid sodium methylate powder that airborne dust is kicked up is easily to human body
And production causes larger harm.
The content of the invention
The present invention provides a kind of solid sodium methylate preparation method, to solve to occur coagulating in existing solid sodium methylate preparation process
The problem of knot.
The present invention provides a kind of solid sodium methylate preparation method, and the preparation method includes：
It is 9 according to mass ratio by liquid methanol sodium and toluene:1-3:1 mix homogeneously, forms mixture a；
The mixture a is warming up to into 95-105 DEG C under conditions of vacuum is 0.075MPa, keeping temperature is constant, holds
Continuous stirring 10-15h, obtains mixture b and methanol；
The mixture b is warming up to into 130-150 DEG C under conditions of vacuum is 0.085MPa, keeping temperature is constant,
6-8h is persistently stirred, solid sodium methylate and toluene is obtained.
In above-mentioned preparation method, toluene can make the methanol in liquid methanol sodium from liquid first in adding liquid methanol sodium
Depart from sodium alkoxide, and methanol can be dissolved completely in toluene solution.By the mixed liquor of toluene and liquid methanol sodium in vacuum
Be 0.075MPa, temperature be 95-105 DEG C under conditions of be dried, methanol can be made to steam from toluene solution.Methanol is steamed
Afterwards, the mixed liquor of only remaining Feldalat NM and toluene, above-mentioned mixed liquor vacuum be 0.085MPa, temperature be 130-150 DEG C
Under the conditions of be dried, as Feldalat NM does not dissolve in toluene, therefore toluene can be completely disengaged from from Feldalat NM, and then obtains powder
Solid sodium methylate.
Further, liquid methanol sodium and the mass ratio of toluene are 9:When 1, prepared solid sodium methylate has higher pure
Degree and preferable stability.
Further, the whipping temp of mixture a be 100 DEG C, mixing time be 12h when, methanol can be completely from mixing
Steam in thing a.When the whipping temp of mixture b is 135 DEG C, mixing time is 8h, toluene can be completely disengaged from from Feldalat NM,
Obtain the solid sodium methylate of powder free from foreign meter.
The technical scheme that embodiments of the invention are provided can include following beneficial effect：
The present invention provides a kind of solid sodium methylate preparation method, and the preparation method includes：By liquid methanol sodium and toluene
It is 9 according to mass ratio:1-3:1 mix homogeneously, forms mixture a；By the mixture a in the condition that vacuum is 0.075MPa
Under be warming up to 95-105 DEG C, keeping temperature is constant, persistently stirs 10-15h, obtains mixture b and methanol；By the mixture b
130-150 DEG C is warming up under conditions of vacuum is 0.085MPa, keeping temperature is constant, persistently stirs 6-8h, obtains solid
Feldalat NM and toluene.Addition of the solid sodium methylate preparation method that the present invention is provided by toluene so that methanol can be from liquid
Completely disengage from out in Feldalat NM and be dissolved completely in toluene solution, and then the gradation of methanol and toluene is realized by step heating
Steam, finally obtain the solid sodium methylate of quality is good.The solid sodium methylate preparation method that the present invention is provided can not only be solved
When in existing process, liquid methanol sodium is dried, viscosity is big, the problem of solid sodium methylate caking, and prepared solid sodium methylate
With total alkali it is high, purity is high, free alkali is low, product specific volume is little and active high the characteristics of, it is adaptable to promote on a large scale with should
With.
It should be appreciated that the general description of the above and detailed description hereinafter are only exemplary and explanatory, not
The present invention can be limited.
Description of the drawings
During accompanying drawing herein is merged in description and the part of this specification is constituted, show the enforcement for meeting the present invention
Example, and be used for explaining the principle of the present invention together with description.
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
Accompanying drawing to be used needed for having technology description is briefly described, it should be apparent that, for those of ordinary skill in the art
Speech, without having to pay creative labor, can be with according to these other accompanying drawings of accompanying drawings acquisition.
Fig. 1 is the schematic flow sheet of solid sodium methylate preparation method provided in an embodiment of the present invention.
Specific embodiment
Here in detail exemplary embodiment will be illustrated, its example is illustrated in the accompanying drawings.Explained below is related to
During accompanying drawing, unless otherwise indicated, the same numbers in different accompanying drawings represent same or analogous key element.Following exemplary embodiment
Described in embodiment do not represent and the consistent all embodiments of the present invention.Conversely, they be only with as appended by
The example of consistent apparatus and method in terms of some described in detail in claims, the present invention.
Accompanying drawing 1 is refer to, accompanying drawing 1 shows the preparation flow of solid sodium methylate preparation method provided in an embodiment of the present invention
Figure.In following specific embodiments, the preparation method of solid sodium methylate is described based on accompanying drawing 1.
Embodiment 1
A kind of solid sodium methylate preparation method is embodiments provided, the preparation method includes：
S101：It is 9 according to mass ratio by liquid methanol sodium and toluene:1 mix homogeneously, forms mixture a；
S102：Mixture a is warming up to into 95 DEG C under conditions of vacuum is 0.075MPa, keeping temperature is constant, is continued
Stirring 12h, obtains mixture b and methanol；
S103：Mixture b is warming up to into 140 DEG C under conditions of vacuum is 0.085MPa, keeping temperature is constant, is continued
Stirring 8h, obtains solid sodium methylate and toluene.
Embodiment 2
A kind of solid sodium methylate preparation method is embodiments provided, the preparation method includes：
S201：It is 3 according to mass ratio by liquid methanol sodium and toluene:1 mix homogeneously, forms mixture a；
S202：Mixture a is warming up to into 105 DEG C under conditions of vacuum is 0.075MPa, keeping temperature is constant, is continued
Stirring 10h, obtains mixture b and methanol；
S203：Mixture b is warming up to into 130 DEG C under conditions of vacuum is 0.085MPa, keeping temperature is constant, is continued
Stirring 6h, obtains solid sodium methylate and toluene.
Embodiment 3
A kind of solid sodium methylate preparation method is embodiments provided, the preparation method includes：
S301：It is 9 according to mass ratio by liquid methanol sodium and toluene:2 mix homogeneously, form mixture a；
S302：Mixture a is warming up to into 100 DEG C under conditions of vacuum is 0.075MPa, keeping temperature is constant, is continued
Stirring 15h, obtains mixture b and methanol；
S303：Mixture b is warming up to into 150 DEG C under conditions of vacuum is 0.085MPa, keeping temperature is constant, is continued
Stirring 8h, obtains solid sodium methylate and toluene.
Embodiment 4
A kind of solid sodium methylate preparation method is embodiments provided, the preparation method includes：
S401：It is 9 according to mass ratio by liquid methanol sodium and toluene:1 mix homogeneously, forms mixture a；
S402：Mixture a is warming up to into 95 DEG C under conditions of vacuum is 0.075MPa, keeping temperature is constant, is continued
Stirring 13h, obtains mixture b and methanol；
S403：Mixture b is warming up to into 135 DEG C under conditions of vacuum is 0.085MPa, keeping temperature is constant, is continued
Stirring 7h, obtains solid sodium methylate and toluene.
The embodiment of the present invention additionally provide the industry standard of the solid sodium methylate prepared by solid sodium methylate preparation method and
Testing result, wherein, the testing result of solid sodium methylate is the testing result of continuous a week, and in one week, sequence number identical is identical
The testing result of time point, concrete industry standard and testing result please refer to Tables 1 and 2 respectively.
Table 1：The industry standard of solid sodium methylate
Table 2：The solid sodium methylate testing result of continuous a week
Contrast Tables 1 and 2 can be derived that, the solid prepared by solid sodium methylate preparation method provided in an embodiment of the present invention
Feldalat NM has good high purity, and meets industry standard, substantially belongs to high-class product.Through the production of continuous one week and inspection
Survey, do not occur industry standard specify outside product, thus, it is possible to illustrate solid sodium methylate provided in an embodiment of the present invention preparation
Method can stablize, it is lasting prepare solid sodium methylate, and the solid sodium methylate for preparing is high-class product.
Those skilled in the art will readily occur to its of the present invention after considering description and putting into practice disclosure of the invention here
Its embodiment.The application is intended to any modification of the present invention, purposes or adaptations, these modifications, purposes or
Person's adaptations follow the general principle of the present invention and including the undocumented common knowledge in the art of the present invention
Or conventional techniques.Description and embodiments are considered only as exemplary, and true scope and spirit of the invention are by following
Claim is pointed out.
It should be appreciated that the precision architecture for being described above and being shown in the drawings is the invention is not limited in, and
And various modifications and changes can be being carried out without departing from the scope.The scope of the present invention is limited only by appended claim.
Claims (4)
1. a kind of solid sodium methylate preparation method, it is characterised in that the preparation method includes：
It is 9 according to mass ratio by liquid methanol sodium and toluene:1-3:1 mix homogeneously, forms mixture a；
The mixture a is warming up to into 95-105 DEG C under conditions of vacuum is 0.075MPa, keeping temperature is constant, persistently stirs
10-15h is mixed, mixture b and methanol is obtained；
The mixture b is warming up to into 130-150 DEG C under conditions of vacuum is 0.085MPa, keeping temperature is constant, is continued
Stirring 6-8h, obtains solid sodium methylate and toluene.
2. solid sodium methylate preparation method according to claim 1, it is characterised in that the liquid methanol sodium and toluene
Mass ratio is 9:1.
3. solid sodium methylate preparation method according to claim 1, it is characterised in that the whipping temp of the mixture a
For 100 DEG C, mixing time is 12h.
4. solid sodium methylate preparation method according to claim 1, it is characterised in that the whipping temp of the mixture b
For 135 DEG C, mixing time is 8h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610943451.8A CN106542967A (en) | 2016-11-02 | 2016-11-02 | A kind of solid sodium methylate preparation method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610943451.8A CN106542967A (en) | 2016-11-02 | 2016-11-02 | A kind of solid sodium methylate preparation method |
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| CN106542967A true CN106542967A (en) | 2017-03-29 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52153904A (en) * | 1976-06-16 | 1977-12-21 | Denki Kagaku Kogyo Kk | Preparation of sodium alkoxide |
| CN1322702A (en) * | 2000-05-10 | 2001-11-21 | 曹衍军 | Technological process producing high-purity sodium alcoholate from liquid sodium alcoholate |
| CN105175224A (en) * | 2015-09-02 | 2015-12-23 | 山东朗恒化学有限公司 | Preparation method of low-residue granular sodium alkoxide or potassium alcoholate |
-
2016
- 2016-11-02 CN CN201610943451.8A patent/CN106542967A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52153904A (en) * | 1976-06-16 | 1977-12-21 | Denki Kagaku Kogyo Kk | Preparation of sodium alkoxide |
| CN1322702A (en) * | 2000-05-10 | 2001-11-21 | 曹衍军 | Technological process producing high-purity sodium alcoholate from liquid sodium alcoholate |
| CN105175224A (en) * | 2015-09-02 | 2015-12-23 | 山东朗恒化学有限公司 | Preparation method of low-residue granular sodium alkoxide or potassium alcoholate |
Non-Patent Citations (2)
| Title |
|---|
| 王勇: "噻唑呋喃类有机锡配合物的合成与性质研究及高纯度固体醇钠（钾）的研制", 《中国优秀博硕士学位论文全文数据库（硕士工程科技Ⅰ辑）》 * |
| 钟友政: "固体甲醇钠的工艺实验室试验研究", 《甲醇设计和生产新技术、甲醇下游产品产业化技术、食品级CO2制备工程技术交流研讨会》 * |
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Application publication date: 20170329 |