CN101139246A - Technique for producing hexabromocyclododecane by atomizing solvent separation method - Google Patents
Technique for producing hexabromocyclododecane by atomizing solvent separation method Download PDFInfo
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- CN101139246A CN101139246A CNA2007101539955A CN200710153995A CN101139246A CN 101139246 A CN101139246 A CN 101139246A CN A2007101539955 A CNA2007101539955 A CN A2007101539955A CN 200710153995 A CN200710153995 A CN 200710153995A CN 101139246 A CN101139246 A CN 101139246A
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- hexabromocyclododecane
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Abstract
The present invention provides a preparation method for hexabromocyclododecane by a spraying and desolventizing method, which belongs to the manufacturing technology field for a chemical product. The technics with the spraying and desolventizing method to produce hexabromocyclododecane is that: the hexabromocyclododecane solution material is prepared by the synthesizing reaction between 1,5,9-cyclododecatriene and bromide under the catalyzing function of tetrabutylammonium bromide in chloroform. The hexabromocyclododecane solution material after being washed, decolored and debromined is to be pumped into the atomizing and desolventizing sprayer; the hexabromocyclododecane is mixed with the water vapor to become fog in the spraying mouth of the sprayer. The flog grain of the hexabromocyclododecane chloroform solution is heater to get rid of the chloroform solution agent to become hexabromocyclododecane solid with the same grain diameter. Because of the gravity function, the grain falls down; the collected hexabromocyclododecane solid flows into a washing kettle provided with the hot water. The hot water is to be milled more to wash off the solution agent. And then after being dried off, the hexabromocyclododecane solid with the same grain diameter is obtained.
Description
Technical field
The present invention relates to a kind of production process of chemical product, particularly technique for producing hexabromocyclododecaby by atomizing solvent separation method.
Technical background
The existing production technique of hexabromocyclododecane is mostly at C
3-C
8The saturated alcohol solvent; in chloroform and isopropylcarbinol mixed solvent diox and the Hydrogen bromide mixed solvent; two-way dropping bromine and 1; 5; 9-cyclododecatriene (cyclododecatriene; CDT) mode of charging; finish bromine and 1; 5; the addition reaction of 9-cyclododecatriene, the paste-like product material of making the suspension of indefinite hexabromocyclododecane particle of size or powder is (referring to United States Patent (USP) 3558727; United States Patent (USP) 4783563; United States Patent (USP) 5004847; United States Patent (USP) 5043492; United States Patent (USP) 6284935 and Chinese patent application numbers 200510041217).This paste-like product material passes through filtration, soda lye wash, oven dry again, according to the service requirements crushing screening, finally makes particle diameter hexabromocyclododecane powder product within the specific limits.
But the industrial goods mass analysis result from market learns: all there are the following problems for the hexabromocyclododecane product of employing aforesaid method and explained hereafter:
Quality index such as the purity of hexabromocyclododecane product and fusing point can not be high.Its reason be in the production process species such as tetrabromo ring dodecylene and hexabromocyclododecane at C
3-C
8In saturated alcohol/chloroform mixed solvent, or the solubleness in Zai diox and the Hydrogen bromide mixed solvent is very low, the product sedimentation rapidly, half-cooked, carry inorganic salt secretly, parcel solvent phenomenon is serious.Though, still can not remove fully being mingled with of hexabromocyclododecane finished product through repeatedly washing process after this.
The hexabromocyclododecane filter cake that leaches after the washing, through overheated cyclone cluster drying and crushing screening, or through bipyramid formula Vacuumdrier drying, pulverizer crushes and screens, and the diameter of particle of gained hexabromocyclododecane finished product distributes and compares broad.
In order to solve 1,5,9-cyclododecatriene, dibromo ring 12 carbon diene, alkene oligomerization and the oligomerisation phenomenon of tetrabromo ring dodecylene in adding the bromine reaction process, it is a kind of effective ways that bromine feeds intake in advance.But bromine shifts to an earlier date charging capacity when big, and bromine is very outstanding to the oxidizing reaction of alcohol.Cause the unit consumption of bromine to increase, it is big that the hexabromocyclododecane production cost becomes.
Summary of the invention
The present invention is directed to hexabromocyclododecane product purity in the above-mentioned industrial production, fusing point, the unequal problem of diameter of particle, propose technique for producing hexabromocyclododecaby by atomizing solvent separation method:
Of the present invention experimental studies have found that: near room temperature, the solubleness of species in the trichloromethane solvent such as tetrabromo ring dodecylene and hexabromocyclododecane are big, and when above, solute can dissolve in solvent the mass ratio of solute and solvent fully at 1: 1.5.So bromine and 1,5, the addition reaction that respectively goes on foot of 9-cyclododecatriene is all carried out in homogeneous phase solution, got rid of fully product in other method half-cooked, carry inorganic salt and parcel solvent phenomenon secretly.
Technique for producing hexabromocyclododecaby by atomizing solvent separation method provided by the invention, it is characterized in that bromine and 1,5, the addition reaction product of 9-cyclododecatriene is the CL state in the trichloromethane solvent, thoroughly remove inorganic salt and completely destroy excess bromine for washing and decolour favourable.
Technique for producing hexabromocyclododecaby by atomizing solvent separation method provided by the invention; it is characterized in that; adopt the water vapor atomization to remove chloroform solvent; and finish granulation or pulverizing process simultaneously; pass through processes such as centrifuge dripping, oven dry again, directly obtain the Powdered or particulate state hexabromocyclododecane finished product that size is certain, size distribution is narrow.
The chloroform solvent rate of recovery of technique for producing hexabromocyclododecaby by atomizing solvent separation method provided by the invention is higher than 95%.
Technique for producing hexabromocyclododecaby by atomizing solvent separation method provided by the invention, it is characterized in that, the production process three wastes only have the hexabromocyclododecane washes, the washes principal pollutant are inorganicss such as Sodium Bromide, sodium hypobromite, yellow soda ash, after the diafiltration purification, capable of circulation applying mechanically do not discharged.
Figure (1) is a technique for producing hexabromocyclododecaby by atomizing solvent separation method schema synoptic diagram provided by the invention.Among the figure (1), 1.CDT storage tank, 2. bromination reaction still, 3. material pump, 4. atomizing precipitation tower, 5. washing still, 6. whizzer, 7. chloroform solvent drainage catheter.
Figure (2) is the atomizing precipitation tower sectional view of technique for producing hexabromocyclododecaby by atomizing solvent separation method provided by the invention.Scheme in (2), 1. chloroform solvent drainage catheter, 2. powder obstruct net, 3. material injector, 4. atomizing precipitation body of the tower, 5. taper connection pipe, 6. steam pipe, 7. materail tube.
Following examples further specify technique for producing hexabromocyclododecaby by atomizing solvent separation method provided by the invention.
Embodiment
Add bromine and desalination bleaching process: get 1,5, the 9-cyclododecatriene places header tank for 280 kilograms.Squeeze into 1600 kilograms of chloroforms in the reactor, drop into 60 kilograms of Tetrabutyl amonium bromides, put into 835 kilograms of bromines.Start reactor and stir, open the reactor coolant valve, keep material in reactor near 30 ℃, with 1,5,9-cyclododecatriene thread is gone in the reactor in 5 hours.Feed in raw material and finish off-response still coolant valve.Carried out slaking 1 hour.Add 150 kilograms of 8% soda ash salt brine solutions in the reactor, stirred 1 hour, tell washing soda salt solution, make the hexabromocyclododecane chloroformic solution.
Spraying desolventizing and finished product operation: in the washing still, inject 1500 kilograms in clear water, open the steam system and the stirring of washing still, keep 95 ℃ of water lotion temperature.Open the coolant system of interchanger on the atomizing precipitation tower.Open the water vapor feed valve of injector on the atomizing precipitation tower, open baiting valve and still bottomspump at the bottom of the still of reactor, be pressed into the hexabromocyclododecane chloroformic solution to atomizing precipitation tower, adjust water vapor feed pressure and hexabromocyclododecane chloroformic solution input speed, make spray effect reach necessary requirement.Hexabromocyclododecane chloroformic solution polishing in the question response still, baiting valve and still bottomspump at the bottom of the still of off-response still.Keep washing still temperature of charge and continue 2 hours for 95 ℃.Close the steam system of the coolant system and the washing still of interchanger on the atomizing precipitation tower.Open the coolant system of washing still,, wait to wash in the still temperature of charge, open the baiting valve at the bottom of the washing still, emit in the washing still material and go into whizzer, carry out centrifuge dripping near 50 ℃ to material cooling in the washing still.Filtrate enters the diffusion cell and handles.Filter cake vacuum-drying gets 1098 kilograms of hexabromocyclododecane finished products, yield 98.5%.Analysis records 179 ℃ of first fusing points, 185 ℃ of heat decomposition temperatures, and the HPLC purity assay is 98.7%, drips a mercury analytical method and measures bromine content 73.9%.
Claims (5)
1. technique for producing hexabromocyclododecaby by atomizing solvent separation method, it is characterized in that, the hexabromocyclododecane chloroformic solution is pumped in the atomizing precipitation tower injector, feed nozzle place and water vapor at injector are mixed into vaporific downward ejection, the hexabromocyclododecane chloroformic solution droplet chloroform solvent that is heated, become the certain hexabromocyclododecane solid of particle diameter, naturally descend by action of gravity, collect in the washing still that hot water is housed, further most solvent is taken off in the heat of stirring water washing, after centrifuge dripping, oven dry, make the technological process of the certain hexabromocyclododecane finished product of particle diameter.
2. be 25～45% according to the hexabromocyclododecane mass percent in the described hexabromocyclododecane chloroformic solution of claim 1.
According to the described steam temperature of claim 1 between 120～140 ℃, water vapor pressure is 0.1～0.4Mpa.
According to the described washing still of claim 1 hot water temperature at 90～98 ℃.
5. comprise that according to the described atomizing precipitation of claim 1 tower body of the tower, chloroform solvent drainage catheter, powder intercept net, material injector, taper connection pipe.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101539955A CN101139246A (en) | 2007-09-18 | 2007-09-18 | Technique for producing hexabromocyclododecane by atomizing solvent separation method |
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| CNA2007101539955A CN101139246A (en) | 2007-09-18 | 2007-09-18 | Technique for producing hexabromocyclododecane by atomizing solvent separation method |
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| CN101139246A true CN101139246A (en) | 2008-03-12 |
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| CNA2007101539955A Pending CN101139246A (en) | 2007-09-18 | 2007-09-18 | Technique for producing hexabromocyclododecane by atomizing solvent separation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106315685A (en) * | 2016-08-23 | 2017-01-11 | 山东国瓷功能材料股份有限公司 | Preparation method and facility of nano manganese-zinc ferrite material |
| CN113582913A (en) * | 2021-08-18 | 2021-11-02 | 河北广祥制药有限公司 | Method for continuously refining nifedipine |
-
2007
- 2007-09-18 CN CNA2007101539955A patent/CN101139246A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106315685A (en) * | 2016-08-23 | 2017-01-11 | 山东国瓷功能材料股份有限公司 | Preparation method and facility of nano manganese-zinc ferrite material |
| CN113582913A (en) * | 2021-08-18 | 2021-11-02 | 河北广祥制药有限公司 | Method for continuously refining nifedipine |
| CN113582913B (en) * | 2021-08-18 | 2023-01-03 | 河北广祥制药有限公司 | Method for continuously refining nifedipine |
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Open date: 20080312 |