CN107556338A - A kind of low taste tricresyl phosphate（The propyl group of 2,3 dichloro 2）The preparation method of ester fire retardant - Google Patents
A kind of low taste tricresyl phosphate（The propyl group of 2,3 dichloro 2）The preparation method of ester fire retardant Download PDFInfo
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Abstract
The present invention relates to fire retardant manufacturing technology field.The invention discloses a kind of low taste tricresyl phosphate (2, the propyl group of 3 dichloro 2) ester fire retardant preparation method, replace butyl titanate of the prior art to participate in reaction using titanium tetrachloride as catalyst, the aftertreatment technology of product crude product is used as using distillation technique and active carbon absorption technology.Tricresyl phosphate (propyl group of 2,3 dichloro 2) Lipase absobed technique has higher combined coefficient in the present invention, generated time was reduced to 18 hours or so by more than 40 hours of prior art；Tricresyl phosphate (propyl group of 2,3 dichloro 2) the ester fire retardant impurity being prepared is less, is colourless transparent oil liquid, peculiar smell is less, and the product after flame-retardant modified will not be made to have unpleasant peculiar smell；Tricresyl phosphate (propyl group of 2,3 dichloro 2) the ester fire retardant being prepared, has the characteristics that good self-extinguishment, lighter color, acid number is low, viscosity is small, can also improve the performances such as the light resistance, water resistance, antistatic and gloss of product.
Description
Technical field
The present invention relates to fire retardant manufacturing technology field, more particularly, to a kind of low taste tricresyl phosphate (2,3- bis- chloro- 2- third
Base) ester fire retardant preparation method.
Background technology
With the development of modernization science and technology, the production of the mankind and living standard improve constantly, synthetic fibers, plastics,
Rubber Polymer material is more and more extensive to be applied in every field, is played in the development of the national economy and people's lives
Great function.But high polymer material is typically all inflammable or flammable, easily triggers fire incident.
In order to solve the problems such as resistance to combustion of synthetic material, suppression cigarette, it is ensured that the security that synthetic material uses, maximally effective side
Method is to add fire retardant.Because fire retardant can be acted on by such as heat-absorbing action, covering, suppress chain reaction, the asphyxia of non-flammable compressive gas
Act on some mechanism and play its fire retardation, combustible material is converted into flame retardant material, reduces substance combustion speed, is prevented
Fire expands.
Tricresyl phosphate (the chloro- 2- propyl group of 1,3- bis-) ester (TDCPP) fire retardant is as halogen-free environment-friendly type flame-proof agent --- organophosphor
The representative of flame retardant, its flame retarding efficiency is high, and volatility is relatively low, oil resistivity and preferable, the chemical name 2 of water-fast drop property, 3- bis-
Chloropropyl phosphate, its molecular formula are C9H15Cl6O4P, product appearance are colourless or pale yellow oily liquid, phosphorus content 7.2%,
Chlorinity 49.4%, viscosity (25 DEG C) 1500 ± 100 centipoises.Its characteristic is dissolved in the organic solvents such as ethanol, chloroform, insoluble in fat
Hydro carbons.
TDCPP is one of anti-flammability and the best kind of persistence in phosphorus chlorine-based flame retardant.Resistance is added in combustible material
Its fire-retardant principle is after combustion agent, and organic phosphorus flame retardant can produce structure more stable crosslinking shape solid matter or carbon when heated
Change layer.On the one hand the formation of carburization zone can prevent polymer from being further pyrolyzed, on the other hand can prevent its internal thermal decomposition production
Biology enters gas phase and participates in combustion process, reaches isolation O2There is heat-insulated, oxygen barrier, prevent fuel gas from outwards escaping,
So as to reach fire-retardant purpose.There are the elements of fire resistance in especially TDCPP containing phosphorus, two kinds of chlorine, thus its flame-retarding characteristic with
The flame-retarding characteristic of both elements is relevant, also causes the increase of its flame retardant effect.
But the production efficiency of tricresyl phosphate (1,3- bis- chloro- 2- propyl group) ester is relatively low in the prior art, is carried out by existing process
Production generally require 40 hours and more than, in production process the raw material reaction time grow, and containing more in obtained product
Incomplete residue and more impurity are reacted, these impurity produce to the quality of tricresyl phosphate (1,3- bis- chloro- 2- propyl group) ester product
Larger adverse effect is given birth to, such as heavier peculiar smell, color and luster are partially yellow, sense organ are influenceed after addition, viscosity is big, is brought not to use
Just, the shortcomings such as acid number is low while also be present, can not meet that the high-performance in industries such as household articles, automobile, high ferro, aircraft industries will
Ask.
The content of the invention
To solve the above problems, the invention provides one kind can greatly shorten process time and obtaining have it is low different
Taste, color and luster are pure, acid number is high, the preparation method of the tricresyl phosphate of modest viscosity (1,3- bis- chloro- 2- propyl group) ester,
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of preparation method of low taste tricresyl phosphate (2,3- bis- chloro- 2- propyl group) ester fire retardant, is comprised the steps of：
A) material preparation of following parts by weight is pressed：2900~3000 parts of POCl3,3750~4000 parts of epoxychloropropane, catalysis
0.8~1.2 part of agent, 100~200 parts of soda ash, 100~200 parts of activated carbon, 800~1200 parts of water；
B) catalyst is added to POCl3；
C) it is slowly added to epoxychloropropane into POCl3 and heats make to be to slowly warm up to 95~105 DEG C, epoxychloropropane adds
Add and be stirred after finishing and be incubated 1.5~2.5 hours；
D) soda ash and water are added into above-mentioned step products and is to slowly warm up to 100~120 DEG C, is followed by stirring for 1~2 hour, stirs
0.5~3 hour is stood after the completion of mixing；
E) remove and contain alkali waste water in product after step d stratification；
F) the product distilation containing alkali waste water will be removed；
G) activated carbon being added into the finished product through distillation processing to handle 1~2 hour, being filtered to remove activated carbon afterwards, low taste is made
Tricresyl phosphate (the chloro- 2- propyl group of 2,3- bis-) ester fire retardant.
In the prior art using the acid number that synthetic product is reduced in lime and by the way of alkali cleaning, but due to the reduction of lime
The ability of acid number is weaker, and the reaction time is also longer so that the time of synthetic product post processing is longer while effect is also bad；This hair
Bright middle use soda ash carries out neutralizing alkali cleaning processing instead of lime, because the activity of soda ash is stronger, it is easier to reacted, and meanwhile it is pure
The water solubility of alkali is also preferable, therefore can greatly reduce processing time using soda ash progress alkali cleaning, the effect of increase alkali cleaning processing
Rate；The discarded buck after alkali cleaning is removed using the method for stratification after alkali cleaning, buck is after sewage treatment facility processing is up to standard
Discharge.
Tricresyl phosphate (the chloro- 2- propyl group of 2,3- bis-) ester that synthesis post processing is obtained using physical method to synthesis in the present invention is thick
Product carry out purification processes, i.e., the impurity in crude product is removed using the method for distillation, can so not change flame-retardant properties
Under the premise of remove crude product in react incomplete impurity, improve the purity of sintetics, it is excellent also make it that final finished has
Colourity and the features such as color and luster；For the peculiar smell in synthesis finished product, the present invention is removed by the way of charcoal absorption, living
Property charcoal have that specific surface area is big, the features such as activity is high, and micropore is flourishing, and decolorizing ability is strong, and pore structure is larger, pore structure is big, energy
There are the various materials larger compared with the color in adsorptive liquid etc., impurity；Activated carbon has very big surface area, and also has in carbon granule
More fine capillaries, this capillary have very strong adsorption capacity, because the surface area of carbon granule is very big, so energy and gas
(impurity) fully contacts, and encounters capillary when these gases (impurity) and is adsorbed, aseptic.
Preferably, catalyst is titanium tetrachloride.
In the technique of conventional synthesis tricresyl phosphate (2,3- bis- chloro- 2- propyl group) ester, using butyl titanate as catalyst, by
In the active relatively low of butyl titanate, the time of synthesis process is longer, generally require 40 hours and more than, production efficiency is very
It is low；After process modification experiment is carried out using other catalyst (such as alchlor and titanium tetrachloride), find to make with titanium tetrachloride
Synthetic reaction the reaction time is carried out for catalyst and shortens nearly half, the reaction time of whole synthesis technique can be foreshortened to
Within 18 hours, but due to titanium tetrachloride and the similar density of tricresyl phosphate (2,3- bis- chloro- 2- propyl group) ester, metatitanic acid can not be used
Four butyl esters remove as the method for catalyst layered, for this difficult point, in the post processing of synthesis technique of the present invention, according to four
The characteristics of boiling point of titanium chloride and tricresyl phosphate (2,3- bis- chloro- 2- propyl group) ester difference is larger, synthesis is removed using the method for distillation
Reacted catalyst impurities, and can also be recycled through distillation processing rear catalyst.
Preferably, activated carbon is mao bamboon preparing active carbon.
Activated carbon uses mao bamboon preparing active carbon in the present invention, and it is raw material by high-quality mao bamboon, through high temperature carbonization, activation and it is more
Kind process is refined to be formed, and compared to normal activated carbon, its capillary structure is more intensive so that and it has bigger specific surface area,
Possessing more powerful adsorption capacity, the gas for producing peculiar smell in sintetics has more preferable adsorption effect, while through inhaling
Attached mao bamboon preparing active carbon can also carry out activating and regenerating.
Preferably, in step c, the adding speed of epoxychloropropane is 20~360kg/h, heating rate is 5~10 DEG C/
h。
Epoxychloropropane if adding speed is too fast can cause that more side reactions occur, cause target as reactant
Products collection efficiency is relatively low, it is therefore desirable to slows down the adding rate of epoxychloropropane, but excessively slow adding rate can also increase reaction
Time, by experiment repeatedly, adding rate is proper in 20~360kg/h, can reduce the generation of side reaction and can also protect
The efficiency of synthesis is demonstrate,proved, when reaction rate is in 20~50kg/h, side reaction less occurs, while the efficiency added is also acceptable
Within the scope of.
Preferably, in step d, heating rate is 5~10 DEG C/h.
Preferably, in step f, the temperature of distilation is 80~150 DEG C.
80~150 DEG C of temperature range is the boiling point section of most of impurity in crude product, is steamed in this silicon carbide
Most impurity can be removed by evaporating processing, while the temperature range is also far below target product tricresyl phosphate (2,3- bis- chloro- 2- third
Base) ester boiling point, the greater loss of target product will not be caused, can ensure to synthesize the yield of target product.
Preferably, in step f during distilation, the heating rate of its temperature rise period is 5~10 DEG C/h.
Therefore, the invention has the advantages that：
(1) tricresyl phosphate (2,3- bis- chloro- 2- propyl group) Lipase absobed technique has higher combined coefficient in the present invention, makes generated time
It was reduced to 18 hours or so by more than 40 hours of prior art；
(1) tricresyl phosphate (2,3- bis- chloro- 2- propyl group) ester fire retardant impurity that the present invention is prepared is less, is water white transparency oily
Liquid, peculiar smell is less, and the product after flame-retardant modified will not be made to have unpleasant peculiar smell；
(2) tricresyl phosphate (2,3- bis- chloro- 2- propyl group) ester fire retardant that the present invention is prepared, there is good self-extinguishment, lighter color, acid
It is worth the features such as low, viscosity is small, can also improves the performances such as the light resistance, water resistance, antistatic and gloss of product.
Embodiment
Technical scheme is further described with reference to embodiment.
Obviously, described embodiment is only the part of the embodiment of the present invention, rather than whole embodiments.Based on this
Embodiment in invention, all other reality that those of ordinary skill in the art are obtained under the premise of creative work is not made
Example is applied, belongs to the scope of protection of the invention.
Embodiment 1
A kind of preparation method of low taste tricresyl phosphate (2,3- bis- chloro- 2- propyl group) ester fire retardant, is comprised the steps of：
A) material preparation of following parts by weight is pressed：2900 parts of POCl3,3750 parts of epoxychloropropane, TiCl 4 catalyst
0.8 part, 100 parts of soda ash, 100 parts of mao bamboon preparing active carbon, 800 parts of water；
B) catalyst is added to POCl3；
C) it is slowly added to epoxychloropropane into POCl3 and heats make to be to slowly warm up to 95 DEG C, epoxychloropropane addition finishes
After be stirred and be incubated 1.5 hours；The adding speed of epoxychloropropane is 20kg/h, and heating rate is 5 DEG C/h；
D) soda ash and water are added into above-mentioned step products and is to slowly warm up to 100 DEG C, is followed by stirring for 1 hour, after the completion of stirring
Stand 0.5 hour；Heating rate is 5 DEG C/h；
E) remove and contain alkali waste water in product after step d stratification；
F) the product distilation containing alkali waste water will be removed；The temperature of distilation is 80 DEG C, and the heating rate of temperature rise period is 5
℃/h；
G) activated carbon being added into the finished product through distillation processing to handle 1 hour, being filtered to remove activated carbon afterwards, low taste phosphoric acid is made
Three (the chloro- 2- propyl group of 2,3- bis-) ester fire retardants.
Embodiment 2
A kind of preparation method of low taste tricresyl phosphate (2,3- bis- chloro- 2- propyl group) ester fire retardant, is comprised the steps of：
A) material preparation of following parts by weight is pressed：2993 parts of POCl3,3892 parts of epoxychloropropane, TiCl 4 catalyst 1
Part, 150 parts of soda ash, 150 parts of mao bamboon preparing active carbon, 1000 parts of water；
B) catalyst is added to POCl3；
C) it is slowly added to epoxychloropropane into POCl3 and heats make to be to slowly warm up to 100 DEG C, epoxychloropropane has added
It is stirred after finishing and is incubated 2 hours；The adding speed of epoxychloropropane is 20kg/h, and heating rate is 7 DEG C/h；
D) soda ash and water are added into above-mentioned step products and is to slowly warm up to 105 DEG C, is followed by stirring for 1.5 hours, stirring is completed
Stand 1 hour afterwards；Heating rate is 7 DEG C/h；
E) remove and contain alkali waste water in product after step d stratification；
F) the product distilation containing alkali waste water will be removed；The temperature of distilation is 110 DEG C, and the heating rate of temperature rise period is
7℃/h；
G) activated carbon being added into the finished product through distillation processing to handle 1.5 hours, being filtered to remove activated carbon afterwards, low taste phosphorus is made
Sour three (the chloro- 2- propyl group of 2,3- bis-) ester fire retardants.
Embodiment 3
A kind of preparation method of low taste tricresyl phosphate (2,3- bis- chloro- 2- propyl group) ester fire retardant, is comprised the steps of：
A) material preparation of following parts by weight is pressed：2950 parts of POCl3,3850 parts of epoxychloropropane, TiCl 4 catalyst
1.1 parts, 160 parts of soda ash, 150 parts of mao bamboon preparing active carbon, 1100 parts of water；
B) catalyst is added to POCl3；
C) it is slowly added to epoxychloropropane into POCl3 and heats make to be to slowly warm up to 100 DEG C, epoxychloropropane has added
It is stirred after finishing and is incubated 2 hours；The adding speed of epoxychloropropane is 200kg/h, and heating rate is 8 DEG C/h；
D) soda ash and water are added into above-mentioned step products and is to slowly warm up to 115 DEG C .5 hours are followed by stirring for, after the completion of stirring
Stand 2 hours；Heating rate is 8 DEG C/h；
E) remove and contain alkali waste water in product after step d stratification；
F) the product distilation containing alkali waste water will be removed；The temperature of distilation is 120 DEG C, and the heating rate of temperature rise period is
8℃/h；
G) activated carbon being added into the finished product through distillation processing to handle 1.5 hours, being filtered to remove activated carbon afterwards, low taste phosphorus is made
Sour three (the chloro- 2- propyl group of 2,3- bis-) ester fire retardants.
Embodiment 4
A kind of preparation method of low taste tricresyl phosphate (2,3- bis- chloro- 2- propyl group) ester fire retardant, is comprised the steps of：
A) material preparation of following parts by weight is pressed：3000 parts of POCl3,4000 parts of epoxychloropropane, TiCl 4 catalyst
1.2 parts, 200 parts of soda ash, 200 parts of mao bamboon preparing active carbon, 1200 parts of water；
B) catalyst is added to POCl3；
C) it is slowly added to epoxychloropropane into POCl3 and heats make to be to slowly warm up to 105 DEG C, epoxychloropropane has added
It is stirred after finishing and is incubated 2.5 hours；The adding speed of epoxychloropropane is 360kg/h, and heating rate is 10 DEG C/h；
D) soda ash and water are added into above-mentioned step products and is to slowly warm up to 120 DEG C, is followed by stirring for 2 hours, after the completion of stirring
Stand 3 hours；Heating rate is 10 DEG C/h；
E) remove and contain alkali waste water in product after step d stratification；
F) the product distilation containing alkali waste water will be removed；The temperature of distilation is 150 DEG C, and the heating rate of temperature rise period is
10℃ /h；
G) activated carbon being added into the finished product through distillation processing to handle 2 hours, being filtered to remove activated carbon afterwards, low taste phosphoric acid is made
Three (the chloro- 2- propyl group of 2,3- bis-) ester fire retardants.
Performance comparison：
The product as made from above-described embodiment and the product of other domestic and international producers are contrasted, it is as a result as follows：
The tricresyl phosphate as made from above-described embodiment (2,3- bis- chloro- 2- propyl group) ester outward appearance is presented it can be seen from the contrast of upper table
Colorless and transparent, color and luster is more excellent, it is seen that impurity therein is less, purer；Acid number is lower, when in use to needing flame retardant treatment
Product has more preferable compatibility；The characteristics of with low taste, because impurity therein is less, its peculiar smell as caused by magazine is more
It is few.Tricresyl phosphate (the chloro- 2- propyl group of 2,3- bis-) the ester preparation method recorded by above-described embodiment prepares tricresyl phosphate (bis- chloro- 2- of 2,3-
Propyl group) ester when the required reaction time it is less, be the 1/4 of prior art, or even shorter, production efficiency is higher.
It should be appreciated that to those skilled in the art, it can according to the above description be improved or be become
Change, and all these modifications and variations should all belong to the protection domain of appended claims of the present invention.
Claims (7)
1. a kind of preparation method of low taste tricresyl phosphate (2,3- bis- chloro- 2- propyl group) ester fire retardant, it is characterised in that include following step
Suddenly：
A) material preparation of following parts by weight is pressed：2900~3000 parts of POCl3,3750~4000 parts of epoxychloropropane, catalysis
0.8~1.2 part of agent, 100~200 parts of soda ash, 100~200 parts of activated carbon, 800~1200 parts of water；
B) catalyst is added to POCl3；
C) it is slowly added to epoxychloropropane into POCl3 and heats make to be to slowly warm up to 95~105 DEG C, epoxychloropropane adds
Add and be stirred after finishing and be incubated 1.5~2.5 hours；
D) soda ash and water are added into above-mentioned step products and is to slowly warm up to 100~120 DEG C, is followed by stirring for 1~2 hour, stirs
0.5~3 hour is stood after the completion of mixing；
E) remove and contain alkali waste water in product after step d stratification；
F) the product distilation containing alkali waste water will be removed；
G) activated carbon being added into the finished product through distillation processing to handle 1~2 hour, being filtered to remove activated carbon afterwards, low taste is made
Tricresyl phosphate (the chloro- 2- propyl group of 2,3- bis-) ester fire retardant.
2. a kind of preparation method of low taste tricresyl phosphate (2,3- bis- chloro- 2- propyl group) ester fire retardant according to claim 1, its
It is characterised by：
Described catalyst is titanium tetrachloride.
3. a kind of preparation method of low taste tricresyl phosphate (2,3- bis- chloro- 2- propyl group) ester fire retardant according to claim 1, its
It is characterised by：
Described activated carbon is mao bamboon preparing active carbon.
4. a kind of preparation method of low taste tricresyl phosphate (2,3- bis- chloro- 2- propyl group) ester fire retardant according to claim 1, its
It is characterised by：
In the step c, the adding speed of epoxychloropropane is 20~360kg/h, and heating rate is 5~10 DEG C/h.
5. a kind of preparation method of low taste tricresyl phosphate (2,3- bis- chloro- 2- propyl group) ester fire retardant according to claim 1, its
It is characterised by：
In the step d, heating rate is 5~10 DEG C/h.
6. a kind of preparation method of low taste tricresyl phosphate (2,3- bis- chloro- 2- propyl group) ester fire retardant according to claim 1, its
It is characterised by：
In the step f, the temperature of distilation is 80~150 DEG C.
A kind of 7. preparation side of low taste tricresyl phosphate (the chloro- 2- propyl group of 2,3- bis-) ester fire retardant according to claim 1 or 6
Method, it is characterised in that：
In the step f during distilation, the heating rate of its temperature rise period is 5~10 DEG C/h.
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| CN108997416A (en) * | 2018-08-28 | 2018-12-14 | 山东泰和水处理科技股份有限公司 | A kind of preparation method of phosphonic acids three (the chloro- 2- propyl of 1,3- bis-) ester |
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| CN109503654A (en) * | 2018-12-28 | 2019-03-22 | 山东泰和水处理科技股份有限公司 | The separation method of catalyst in a kind of esterification system |
| CN110511238A (en) * | 2019-09-17 | 2019-11-29 | 南京师范大学镇江创新发展研究院 | A kind of adion liquid catalyst reduces the separation method of product acid value |
| CN110818736A (en) * | 2019-10-30 | 2020-02-21 | 南京师范大学镇江创新发展研究院 | Method for removing Lewis acid ionic liquid catalyst in phosphate ester flame retardant product |
| CN114478620A (en) * | 2022-02-23 | 2022-05-13 | 淮安晨化新材料有限公司 | Preparation process of odorless phosphate flame retardant |
| CN114478620B (en) * | 2022-02-23 | 2024-03-22 | 淮安晨化新材料有限公司 | Preparation process of odorless phosphate flame retardant |
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Denomination of invention: Preparation method of low taste tri (2,3-dichloro-2-propyl) phosphate flame retardant Effective date of registration: 20221024 Granted publication date: 20190611 Pledgee: Zhejiang Suichang Rural Commercial Bank Co.,Ltd. Pledgor: ZHEJIANG HONGHAO TECHNOLOGY CO.,LTD. Registration number: Y2022330002781 |