CN108180700B - 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
- CN108180700B CN108180700B CN201711400898.1A CN201711400898A CN108180700B CN 108180700 B CN108180700 B CN 108180700B CN 201711400898 A CN201711400898 A CN 201711400898A CN 108180700 B CN108180700 B CN 108180700B
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- Prior art keywords
- solid powder
- organic solid
- desiccant
- drying means
- molecular sieve
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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
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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
- 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
Abstract
The present invention discloses a kind of drying means of easily distillation organic solid powder, includes the following steps: that (1) is added and the segregative desiccant 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 simultaneously, and keeps certain time；(3) solid powder after drying is sieved, removes desiccant.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, effect is obvious.
Description
Technical field
The invention belongs to dry fields, are related to the drying means more particularly to three second of a kind of easily distillation organic solid powder
The drying means of alkene diamines and piperazine.
Background technique
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 it is 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 formation crystalline hydrate, and easily distil.
Therefore, in dry field, in the prior art, it is difficult using means such as high temperature drying, vacuum drying and freeze-dryings to easy distillation
Its water content is effectively reduced while keeping product high yield in solid powder.And water law is removed by chemical seasoning, such as azeotropic essence
Method, at high cost, complex process are evaporated, and inevitably introduces other organic impurities；Using passing through disclosed in CN103836885
Introduce the side for metal organic salt (such as: trimethyl gallium, trimethyl aluminium, trimethyl indium) the chemistry water removal that there is strong reactivity with water
Method may introduce the metal impurities such as gallium, aluminium, indium, to influence final product quality.
Summary of the invention
The technical problem to be solved by the present invention is to for the dry difficult technology of organic solid powder that easily distils in the prior art
Problem provides a kind of simple and easy 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) desiccant is added into the container for being placed with easy distillation organic solid powder, and has desiccant with easy distillation
Machine solid powder is sufficiently mixed uniformly；The desiccant is with water with strong physical adsorption property and with regular morphology and size
Solid particle, wherein compression strength >=20N, rate of wear≤0.1%, pattern is spherical shape, bar shaped, annular or cloverleaf pattern,
Particle size >=2mm；The desiccant is selected from one of molecular sieve, silica gel and porous aluminas or a variety of；The easy distillation has
Sublimation temperature≤80 DEG C of machine solid powder；Desiccant additional amount is 6~20 times easily to distil organic solid powder containing water quality；
(2) it is passed through dry gas into container and heats simultaneously, keep 2~12h；Wherein Jia Rewendu≤60 DEG C；It (3) will be after drying
Solid powder sieving, removes desiccant.
Desiccant 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 desiccant with will not be damaged in the drying process of easy-sublimation solid powder, and
Can be ensured after drying desiccant with it is easily separated by drying solid powder, while new impurity will not be introduced.
Desiccant of the present invention can be selected from molecular sieve, including 3A, 4A, 5A, 13X and silica gel, porous aluminas
It is one or more, preferably one of 3A molecular sieve, 4A molecular sieve, 13X molecular sieve and silica gel or a variety of, further preferably 4A molecular sieve
And one or both of silica gel.
In addition to this, on the basis of ensureing compression strength and rate of wear, desiccant 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 desiccant well contacted with by dried powder and product separation process in desiccant hold with by dried powder
Segregative particle size and pattern are also allowed.
Desiccant, desiccant additional amount at least phase is added into the container for being placed with easy distillation organic solid powder in the present invention
When 6~20 times in 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, is 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 it is lower to work as heating temperature, or even not heated also possible but dry
The dry time extends, this is understandable.Heating time 2~12 hours in the present invention, preferably 2~8 hours.In drying process
In, it is passed through dry gas into container, to reduce the vapour pressure of water in container, or vacuum means is 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.
Drying of the present invention applied to the easy distillation organic solid powder of sublimation temperature≤80 DEG C, including triethylene diamine,
Piperazine, 2,5- lupetazin, 2,6-dimethyl-piperizine etc., preferably one of triethylene diamine and piperazine.
The present invention removes desiccant particle by the means of sieving from by drying solid powder, and the desiccant after absorbing water
Particle regenerates in such a way that steam heats or routinely roasts, so that the purpose that desiccant is reused can be realized.
Compared with complicated, at high cost with prior art processes, the beneficial effects of the invention are as follows for easily distillation organic solid powder
The dry difficult technical problem in end provides a kind of simple process, the dry water-eliminating method of easy distillation organic solid powder 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
Taking 10g water content is 13.2% triethylene diamine solid powder, and air blast is simultaneously heated under the conditions of 40 DEG C, periodically taken
Sample, analysis, is tested, data are as follows through karl Fischer titrator:
| Time/h | 1 | 2 | 3 |
| Water content/% | 13.3 | 13.8 | 13.7 |
Embodiment 1
Taking 100g water content is 13.2% triethylene diamine solid powder, the 4A molecular sieve after 130g high-temperature activation is added
Ball is uniformly mixed, heats under the conditions of 40 DEG C, be passed through high pure nitrogen and stand 2h, then the solid powder after drying is sieved, sieve
Fall 4A molecular sieve spheres.
It is tested through karl Fischer moisture teller, uses triethylene diamine water content obtained by this method for 0.11%.
Embodiment 2
Taking 100g water content is 13.2% triethylene diamine solid powder, the 4A molecular sieve after 300g high-temperature activation is added
Ball is uniformly mixed, heats under the conditions of 40 DEG C, be passed through high-purity argon gas and stand 2h, then the solid powder after drying is sieved, sieve
Fall 4A molecular sieve spheres.
It is tested through karl Fischer moisture teller, uses triethylene diamine water content obtained by this method for 0.18%.
Embodiment 3
Taking 100g water content is 13.2% triethylene diamine solid powder, and 260g discoloration silica-gel sphere is added, is uniformly mixed,
It is heated under the conditions of 36 DEG C, be passed through high pure nitrogen and stand 3h, then the solid powder after drying is sieved, remove discoloration silica gel
Ball.
It is tested through karl Fischer moisture teller, uses triethylene diamine water content obtained by this method for 0.21%.
Embodiment 4
Taking 200g water content is 14.8% piperazine solid powder, and the 4A molecular sieve spheres after 600g high-temperature activation is added are mixed
It closes uniformly, 3h is heated and stood under the conditions of 45 DEG C, then the solid powder after drying is sieved, remove 4A molecular sieve spheres.
It is tested through karl Fischer moisture teller, uses piperazine water content obtained by this method for 0.08%.
Embodiment 5
Taking 100g water content is 14.8% piperazine solid powder, and the 4A molecular sieve spheres after 200g high-temperature activation is added are mixed
It closes uniformly, is heated under the conditions of 42 DEG C, be passed through high pure nitrogen and stand 2h, then the solid powder after drying is sieved, remove 4A
Molecular sieve spheres.
It is tested through karl Fischer moisture teller, uses piperazine water content obtained by this method for 0.10%.
Conclusion: the present invention substantially increases the drying effect to easy-sublimation solid powder, and simple 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 easily distillation organic solid powder, includes the following steps:
(1) to be placed with easily distillation organic solid powder container in desiccant is added, and make desiccant with easily distil it is organic solid
Body powder is sufficiently mixed uniformly；The desiccant is with water with strong physical adsorption property and consolidating with regular morphology and size
Body particle, wherein compression strength >=20N, rate of wear≤0.1%, pattern are spherical shape, bar shaped, annular or cloverleaf pattern, particle size
≥2mm；The desiccant is selected from one of molecular sieve, silica gel and porous aluminas or a variety of；The easy distillation organic solid
Powder is the organic matter of sublimation temperature≤80 DEG C；Desiccant additional amount is 6 ~ 20 easily to distil organic solid powder containing water quality
Times；
(2) it is passed through dry gas into container and heats simultaneously, keep 2 ~ 12h；Wherein Jia Rewendu≤60 DEG C；
(3) solid powder after drying is sieved, removes desiccant.
2. the drying means of easy distillation organic solid powder according to claim 1, which is characterized in that the easy distillation has
Machine solid powder is one of 2,5- lupetazin or 2,6- lupetazin.
3. the drying means of easy distillation organic solid powder according to claim 1, which is characterized in that desiccant additional amount
10 times for the organic solid powder that easily distils containing water quality.
4. the drying means of easy distillation organic solid powder according to claim 1, which is characterized in that molecular sieve is selected from
One of 3A, 4A, 5A, 13X or a variety of.
5. the drying means of easy distillation organic solid powder according to claim 1, which is characterized in that desiccant is selected from 3A
One of molecular sieve, 4A molecular sieve, 13X molecular sieve and silica gel are a variety of.
6. the drying means of easy distillation organic solid powder according to claim 1, which is characterized in that desiccant is selected from 4A
One or both of molecular sieve and silica gel.
7. the drying means of easy distillation organic solid powder according to claim 1, which is characterized in that the easy distillation has
Machine solid powder is one of triethylene diamine or piperazine.
8. the drying means of easy distillation organic solid powder according to claim 1, which is characterized in that Jia Rewendu≤45
DEG C, keep 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 |
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| 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 |
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| CN108180700A CN108180700A (en) | 2018-06-19 |
| CN108180700B true CN108180700B (en) | 2019-11-22 |
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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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| CN112916594B (en) * | 2021-05-10 | 2021-07-27 | 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 |
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| CN108180700A (en) | 2018-06-19 |
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