CN103224523A - Preparation method of tricresyl phosphate T306 - Google Patents
Preparation method of tricresyl phosphate T306 Download PDFInfo
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- CN103224523A CN103224523A CN 201310120627 CN201310120627A CN103224523A CN 103224523 A CN103224523 A CN 103224523A CN 201310120627 CN201310120627 CN 201310120627 CN 201310120627 A CN201310120627 A CN 201310120627A CN 103224523 A CN103224523 A CN 103224523A
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- filtrating
- tricresyl phosphate
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- tritolyl phosphate
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Abstract
The present invention relates to a preparation method of tricresyl phosphate T306, which includes the following steps of (1) bleaching and removing phenol: evenly adding 0.5-0.8wt% of adsorbent-801 and 0.4-0.6wt% of antioxidant-1010, evenly mixing at the temperature of 65+/- 2DEG C, cycling for 6 to 8 hours; (2) precisely filtrating: filtrating the mixture with the filter of 50 to 70 meshes, pressurized filtrating to be in line with the index to obtain the T306. The invention provides a method for refining tricresyl phosphate T306, which discovers the adsorbent and the antioxidant suitable for purifying TCP through repeated research, and the index of existing products refined by the method meets the requirements of Table 1. The fire-retardant property of existing products at home and abroad is increased and the application is expanded, which greatly improve the application field of domestic fire-retardants.
Description
Technical field
The invention belongs to flame retardant area, especially a kind of method for preparing Tritolyl Phosphate T306.
Background technology
The oxygen compound that contains trace in the processed oil of existing phosphoric acid ester, picture mainly is that to meet that direct metal contact when existing be exactly that chemical reaction generation salt takes place to the floating type of the list of organic acid and phenol, the metallic surface is corroded, existence just because of the few part of this class, and can influence use properties as T306, shorten its work-ing life, therefore, it is deleterious containing oxygen compound, should from finished product, remove or be restricted in the optimality criterion, to stablize and to prolong its work-ing life, in addition, the observed mechanical impurity of the difficulty or ease in the finished product phosphoric acid ester, be meant and be present in that all are insoluble to the precipitation state of solvent or the material of suspended state among the superfine product T306, for these impurity substances, be visible, be can be by 80～100 ears close to removing by filter; But some impurity is that some are sightless, is the atomic organic composition that is insoluble to solvent, if any atomic carbide of very micro-carbene and the residual drop of rectifying etc.; These impurity divide by form, minimum solid particulate state is arranged, as have or not coloured residual bits matter foreign particle etc., dissolved state is also arranged, residual and a spot of slag particle etc. as the various additives that add and sorbent material etc., be be difficult for to see the trace of finding to be in emulsified state or water white in addition, as silicone grease and monoester oil and purification agent etc., these all greatly influence the effect of Tritolyl Phosphate as siliceous material.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, the method for preparing Tritolyl Phosphate T306 of a kind of purity height, stable in properties is provided.
The present invention realizes that the technical scheme of purpose is as follows:
A kind of method for preparing Tritolyl Phosphate T306, step is as follows:
⑴ decolour, remove phenol: sorbent material-801, and oxidation inhibitor-1010, add-on oxidation inhibitor 0.4-0.6%, 65+-2 ℃ of sorbent material 0.5-0.8% stirs, circulation 6-8 hour;
⑵ secondary filter: use 50-70 order strainer to filter, pressure filtration finishes to be T306 after meeting index.
And described added quantity of antioxidant is 0.4-0.6wt%.
And described sorbent material add-on is 0.5-0.8wt%.
Advantage of the present invention and beneficial effect are:
The invention provides a kind of process for purification of Tritolyl Phosphate, by research and development repeatedly, the sorbent material and the oxidation inhibitor of TCP purifying have been found to adapt to, after currently available products is made with extra care by present method, its index reaches the described every requirement of table 1, owing to domestic and international currently available products, has increased the flame retardant properties of this product, enlarged the use range of this product, the very big Application Areas of having improved domestic fire retardant.
Embodiment
Below in conjunction with embodiment, following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Raw material, commercially available TCP, usual production.
A kind of method for preparing Tritolyl Phosphate T306, step is as follows:
⑴ decolour, remove phenol: sorbent material-801, and oxidation inhibitor-1010, add-on oxidation inhibitor 0.4-0.6wt%, 65 ± 2 ℃ of sorbent material 0.5-0.8wt% stir, circulating reaction 6-8 hour;
⑵ secondary filter: use 50-70 order strainer to filter pressure filtration.
Detect index and whether meet following standard,, repeat above-mentioned steps ⑴ and ⑵ again if do not meet.
The Tritolyl Phosphate T306 technical requirements of the refining back of table 1
| Index name | Index |
| Outward appearance | The limpid thick liquid of water white transparency |
| Color and luster (CRe-Co)≤ | 50 |
| Proportion D 20 | 1.168～1.180 |
| Suan Zhi ㎎ KOH/g≤ | 0.080 |
| Flash-point ℃ (opening) 〉= | 235 |
| Granularity AEA-6D level≤ | 6 |
| Free phenol %≤ | 0.080 |
| Moisture content ppm≤ | 300 |
| Muriate %≤ | 0.010 |
Claims (3)
1. method for preparing Tritolyl Phosphate T306, it is characterized in that: step is as follows:
⑴ decolouring, remove phenol: sorbent material-801, oxidation inhibitor-1010,65 ± 2 ℃ stirs circulation 6-8 hour;
⑵ secondary filter: use 50-70 order strainer to filter, be T306 after meeting index.
2. the method for preparing Tritolyl Phosphate T306 according to claim 1 is characterized in that: described added quantity of antioxidant is 0.4-0.6wt%.
3. the method for preparing Tritolyl Phosphate T306 according to claim 1 is characterized in that: described sorbent material add-on is 0.5-0.8wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310120627 CN103224523A (en) | 2013-04-09 | 2013-04-09 | Preparation method of tricresyl phosphate T306 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310120627 CN103224523A (en) | 2013-04-09 | 2013-04-09 | Preparation method of tricresyl phosphate T306 |
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| CN103224523A true CN103224523A (en) | 2013-07-31 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 201310120627 Pending CN103224523A (en) | 2013-04-09 | 2013-04-09 | Preparation method of tricresyl phosphate T306 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109593099A (en) * | 2017-09-30 | 2019-04-09 | 中国石油天然气股份有限公司 | Preparation method of high-purity tricresyl phosphate |
-
2013
- 2013-04-09 CN CN 201310120627 patent/CN103224523A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109593099A (en) * | 2017-09-30 | 2019-04-09 | 中国石油天然气股份有限公司 | Preparation method of high-purity tricresyl phosphate |
| CN109593099B (en) * | 2017-09-30 | 2021-04-30 | 中国石油天然气股份有限公司 | Preparation method of high-purity tricresyl phosphate |
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