CN108180700A - A kind of drying means of easy distillation organic solid powder - Google Patents
A kind of drying means of easy distillation organic solid powder Download PDFInfo
- Publication number
- CN108180700A CN108180700A CN201711400898.1A CN201711400898A CN108180700A CN 108180700 A CN108180700 A CN 108180700A CN 201711400898 A CN201711400898 A CN 201711400898A CN 108180700 A CN108180700 A CN 108180700A
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- China
- Prior art keywords
- solid powder
- organic solid
- drier
- drying means
- distillation organic
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- 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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Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/16—Drying solid materials or objects by processes not involving the application of heat by contact with sorbent bodies, e.g. absorbent mould; by admixture with sorbent materials
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/06—Controlling, e.g. regulating, parameters of gas supply
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/06—Controlling, e.g. regulating, parameters of gas supply
- F26B21/10—Temperature; Pressure
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
- F26B25/001—Handling, e.g. loading or unloading arrangements
- F26B25/002—Handling, e.g. loading or unloading arrangements for bulk goods
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Molecular Biology (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Drying Of Gases (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The present invention discloses a kind of drying means of easy distillation organic solid powder, includes the following steps：(1) it is added in and the segregative drier of solid powder into the container for being placed with the organic solid powder that easily distils；(2) heating is simultaneously passed through dry inert gas into container, and kept for certain time simultaneously；(3) dried solid powder is sieved, removes drier.Present invention process is simple, at low cost, applied to the drying of easy distillation organic solid powder, is particularly applied to the drying process of triethylene diamine and piperazine, with obvious effects.
Description
Technical field
The invention belongs to dry fields, are related to a kind of drying means more particularly to three second of easy distillation organic solid powder
The drying means of alkene diamines and piperazine.
Background technology
Triethylene diamine is that one kind is widely used in polyurethane, plastics, pesticide and electroplating industry and as effective catalyst
Important organic chemical industry's product as vinyl polymerization and ethylene oxide polymerized hydrocarbon.Meanwhile piperazine be also one kind be widely used in antibacterial,
The synthesis of the drugs such as treating tuberculosis, decompression, hypoglycemic, sedation-analgesia and applied to preservative, antioxidant, stabilizer, surface
The weight in the fields such as activating agent, corrosion inhibiter, foaming agent, vulcanization accelerator, coating, pesticide, leather, fiber, wastewater treatment and carbon sequestration
Want organic intermediate.
However both Organic chemical products all have extremely strong hygroscopicity, easily form crystalline hydrate, and easily distil.
Therefore, in dry field, it is difficult to easily distilling the means such as in the prior art, to dry, be dried in vacuo and be freeze-dried using high temperature
Solid powder effectively reduces its water content while product is kept in high yield.And by chemical seasoning except water law, such as azeotropic essence
Method, of high cost, complex process are evaporated, and inevitably introduces other organic impurities；Using passing through disclosed in CN103836885
Introduce the metal organic salt that there is strong reactivity with water (such as：Trimethyl gallium, trimethyl aluminium, trimethyl indium etc.) chemistry water removal side
Method may introduce the metal impurities such as gallium, aluminium, indium, so as to influence final product quality.
Invention content
The technical problem to be solved by the present invention is to be directed in the prior art the easily difficult technology of distillation organic solid powder drying
Problem provides a kind of simple and practicable easy distillation organic solid powder drying water-eliminating method, especially triethylene diamine and piperazine
Drying water-eliminating method.
A kind of easily distillation organic solid powder drying method provided by the present invention, includes the following steps：
(1) drier is added in into the container for being placed with easy distillation organic solid powder, and drier is made to have with easily distillation
Machine solid powder is sufficiently mixed uniformly；The drier is with strong physical absorption performance and with regular morphology and size with water
Solid particle, wherein compression strength >=20N, rate of wear≤0.1%, pattern be spherical shape, bar shaped, annular or cloverleaf pattern,
Particle size >=2mm；The drier is one or more in molecular sieve, silica gel and Woelm Alumina；The easy distillation has
Sublimation temperature≤80 DEG C of machine solid powder；Drier addition is 6~20 times of easily distillation organic solid powder containing water quality；
(2) while into container it is passed through dry gas and heats, keep 2~12h；Wherein Jia Rewendu≤60 DEG C；It (3) will be dried
Solid powder is sieved, and removes drier.
Drier compression strength >=20N of the present invention, rate of wear≤0.1%.Wherein, compression strength and rate of wear include
But be not limited to range above, if the drier with will not be damaged in the drying process of easy-sublimation solid powder, and
Drier can be ensured after drying with easily separated by drying solid powder, while new impurity will not be introduced.
Drier of the present invention may be selected from molecular sieve, including in 3A, 4A, 5A, 13X and silica gel, Woelm Alumina
It is one or more, preferably one or more in 3A molecular sieves, 4A molecular sieves, 13X molecular sieves and silica gel, further preferably 4A molecular sieves
And one or both of silica gel.
In addition to this, on the basis of compression strength and rate of wear is ensured, drier is with regular morphology and size
Solid particle, such as spherical shape, bar shaped, annular or cloverleaf pattern, particle size >=2mm.But the present invention is not limited to range above, only
Will in the drying process drier with by drier in dried powder good contact and product separation process with being held by dried powder
Segregative particle size and pattern are also allowed.
The present invention adds in drier, drier addition at least phase into the container for being placed with easy distillation organic solid powder
When in 6~20 times of easily distillation organic solid powder containing water quality, preferably 10 containing water quality times.
Heating temperature is less than or equal to 60 DEG C in the present invention, preferably smaller than equal to 45 DEG C.Really, what the present invention utilized is different
Principle is removed water in the physical absorption of chemical reaction water removal, therefore when heating temperature is lower, do not heat even also possible but dry
Dry time lengthening, this is understandable.Heating time 2~12 hours in the present invention, preferably 2~8 hours.In drying process
In, dry gas is passed through into container, to reduce the vapour pressure of water in container or vacuum means used to accelerate drying efficiency,
All it is allowed.In view of process costs, it is the most suitable to be passed through dry inert gas, wherein dry gas can be selected nitrogen,
Argon gas etc..In the present invention, especially for the drying of triethylene diamine and piperazine, as long as without using being chemically reacted with the two
Gas medium all may be used.
The present invention is applied to the drying of the easy distillation organic solid powder of sublimation temperature≤80 DEG C, including triethylene diamine,
One kind in piperazine, 2,5- lupetazins, 2,6-dimethyl-piperizine etc., preferably triethylene diamine and piperazine.
The present invention removes desiccant particle by the means of sieving from by drying solid powder, and the drier after absorbing water
Particle regenerates in a manner that steam heats or routinely roasts, so as to realize the purpose of drier reuse.
With prior art processes it is complicated, it is of high cost compared with, the beneficial effects of the invention are as follows for easy distillation organic solid powder
The technical issues of end is dry difficult provides a kind of easy distillation organic solid powder drying water-eliminating method simple for process, at low cost.It adopts
With the method for the present invention, triethylene diamine water content can be reduced to 0.11%, and piperazine water content can be down to 0.08%.
Specific embodiment
Below in conjunction with specific embodiment, the invention will be further described.It should be understood that these embodiments are merely to illustrate this
It invents rather than limits the scope of the invention.In addition, it should also be understood that, upon reading this disclosure, those skilled in the art can be with
The present invention is made various changes or modifications, such equivalent forms equally fall within limited range of the present invention.
Control group
The triethylene diamine solid powder that 10g water content is 13.2% is taken, air blast is simultaneously heated under the conditions of 40 DEG C, periodically taken
Sample, analysis are tested through karl Fischer titrator, and data are as follows：
| Time/h | 1 | 2 | 3 |
| Water content/% | 13.3 | 13.8 | 13.7 |
Embodiment 1
The triethylene diamine solid powder that 100g water content is 13.2% is taken, adds in the 4A molecular sieves after 130g high-temperature activations
Ball is uniformly mixed, is heated under the conditions of 40 DEG C, be passed through high pure nitrogen and stand 2h, then dried solid powder is sieved, and sieves
Fall 4A molecular sieve spheres.
It is tested through karl Fischer moisture teller, uses triethylene diamine water content obtained by this method as 0.11%.
Embodiment 2
The triethylene diamine solid powder that 100g water content is 13.2% is taken, adds in the 4A molecular sieves after 300g high-temperature activations
Ball is uniformly mixed, is heated under the conditions of 40 DEG C, be passed through high-purity argon gas and stand 2h, then dried solid powder is sieved, and sieves
Fall 4A molecular sieve spheres.
It is tested through karl Fischer moisture teller, uses triethylene diamine water content obtained by this method as 0.18%.
Embodiment 3
The triethylene diamine solid powder that 100g water content is 13.2% is taken, 260g discoloration silica-gel spheres is added in, is uniformly mixed,
It is heated under the conditions of 36 DEG C, be passed through high pure nitrogen and stand 3h, then dried solid powder is sieved, remove discoloration silica gel
Ball.
It is tested through karl Fischer moisture teller, uses triethylene diamine water content obtained by this method as 0.21%.
Embodiment 4
The piperazine solid powder that 200g water content is 14.8% is taken, adds in the 4A molecular sieve spheres after 600g high-temperature activations, is mixed
It closes uniformly, is heated under the conditions of 45 DEG C and stand 3h, then dried solid powder is sieved, remove 4A molecular sieve spheres.
It is tested through karl Fischer moisture teller, uses piperazine water content obtained by this method as 0.08%.
Embodiment 5
The piperazine solid powder that 100g water content is 14.8% is taken, adds in the 4A molecular sieve spheres after 200g high-temperature activations, is mixed
It closes uniformly, is heated under the conditions of 42 DEG C, be passed through high pure nitrogen and stand 2h, then dried solid powder is sieved, remove 4A
Molecular sieve spheres.
It is tested through karl Fischer moisture teller, uses piperazine water content obtained by this method as 0.10%.
Conclusion：The present invention substantially increases the drying effect to easy-sublimation solid powder, and simple for process, at low cost.It adopts
With the method for the present invention, triethylene diamine water content can be reduced to 0.11%, and piperazine water content can be down to 0.08%.
Claims (8)
1. a kind of drying means of easy distillation organic solid powder, includes the following steps：
(1) drier is added in, and make drier organic solid with easily distilling into the container for being placed with easy distillation organic solid powder
Body powder is sufficiently mixed uniformly；The drier is consolidating with strong physical absorption performance and with regular morphology and size with water
Body particle, wherein compression strength >=20N, rate of wear≤0.1%, pattern be spherical shape, bar shaped, annular or cloverleaf pattern, particle ruler
Very little >=2mm；The drier is one or more in molecular sieve, silica gel and Woelm Alumina；It is described easily distil it is organic solid
Body powder is the organic matter of sublimation temperature≤80 DEG C；Drier addition for easily distillation organic solid powder containing water quality 6~
20 times；(2) while into container it is passed through dry gas and heats, keep 2~12h；Wherein Jia Rewendu≤60 DEG C；It (3) will be dry
Solid powder sieving after dry, removes drier.
2. according to the drying means of claim 1 easily distillation organic solid powder, which is characterized in that the easy distillation organic solid
Powder is one kind of triethylene diamine, piperazine, 2,5- lupetazins or 2,6- lupetazins.
3. according to the drying means of claim 1 easily distillation organic solid powder, which is characterized in that drier addition is easily rises
10 times containing water quality of magnificent organic solid powder.
4. according to claim 1 easily distillation organic solid powder drying means, which is characterized in that molecular sieve be selected from 3A, 4A,
It is one or more in 5A, 13X.
5. according to the drying means of claim 1 easily distillation organic solid powder, which is characterized in that drier is selected from 3A molecules
It is one or more in sieve, 4A molecular sieves, 13X molecular sieves and silica gel.
6. according to the drying means of claim 1 easily distillation organic solid powder, which is characterized in that drier is selected from 4A molecular sieves
And one or both of silica gel.
7. according to the drying means of claim 1 easily distillation organic solid powder, which is characterized in that the easy distillation organic solid
Powder is one kind in triethylene diamine or piperazine.
8. according to the drying means of claim 1 easily distillation organic solid powder, which is characterized in that Jia Rewendu≤45 DEG C are protected
Hold 2~8h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711400898.1A CN108180700B (en) | 2017-12-22 | 2017-12-22 | A kind of drying means of easy distillation organic solid powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711400898.1A CN108180700B (en) | 2017-12-22 | 2017-12-22 | A kind of drying means of easy distillation organic solid powder |
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| Publication Number | Publication Date |
|---|---|
| CN108180700A true CN108180700A (en) | 2018-06-19 |
| CN108180700B CN108180700B (en) | 2019-11-22 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201711400898.1A Active CN108180700B (en) | 2017-12-22 | 2017-12-22 | A kind of drying means of easy distillation organic solid powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112916594A (en) * | 2021-05-10 | 2021-06-08 | 中国科学院过程工程研究所 | Anti-condensation method in dry-method carbide slag recycling process |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004112422A2 (en) * | 2003-06-06 | 2004-12-23 | Bernard Jay Greenspan | Hearing aid dryer |
| CN102342565A (en) * | 2011-09-28 | 2012-02-08 | 福建农林大学 | Combined drying method |
| CN103640108A (en) * | 2013-12-14 | 2014-03-19 | 甘肃银光聚银化工有限公司 | Method for drying polycarbonate |
| CN103808108A (en) * | 2013-11-19 | 2014-05-21 | 浙江祥邦科技有限公司 | Low-temperature drying method of low-melting-point resin |
| CN103822442A (en) * | 2014-02-17 | 2014-05-28 | 河南科技大学 | Method for drying honeysuckles |
| CN106766676A (en) * | 2016-12-20 | 2017-05-31 | 西北稀有金属材料研究院 | A kind of drying means of tin oxide precursor powder |
-
2017
- 2017-12-22 CN CN201711400898.1A patent/CN108180700B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004112422A2 (en) * | 2003-06-06 | 2004-12-23 | Bernard Jay Greenspan | Hearing aid dryer |
| CN102342565A (en) * | 2011-09-28 | 2012-02-08 | 福建农林大学 | Combined drying method |
| CN103808108A (en) * | 2013-11-19 | 2014-05-21 | 浙江祥邦科技有限公司 | Low-temperature drying method of low-melting-point resin |
| CN103640108A (en) * | 2013-12-14 | 2014-03-19 | 甘肃银光聚银化工有限公司 | Method for drying polycarbonate |
| CN103822442A (en) * | 2014-02-17 | 2014-05-28 | 河南科技大学 | Method for drying honeysuckles |
| CN106766676A (en) * | 2016-12-20 | 2017-05-31 | 西北稀有金属材料研究院 | A kind of drying means of tin oxide precursor powder |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112916594A (en) * | 2021-05-10 | 2021-06-08 | 中国科学院过程工程研究所 | Anti-condensation method in dry-method carbide slag recycling process |
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| Publication number | Publication date |
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| CN108180700B (en) | 2019-11-22 |
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