- Single-crystal structure analysis of a novel aryl phosphinate diglycidyl ether
-
The crystal structure of 10-[2,5-bis(2,3-epoxy-1-propoxy)phenyl]-9-oxa-10-phosphaphenanthren-10-one has been studied by single-crystal X-ray diffraction. The unit cell of C24H21O6P, Mr = 436.4, is triclinic, P1, with a = 8.507 (3), b = 10.613 (4), c = 12.457 (3) A, α = 80.05 (3), β = 71.38 (2), γ = 76.69 (3)°, V = 1031.1 (6) A3, Z = 2, Dx = 1.406 Mg m-3 and μ(Mo Kα) = 0.17 mm-1. The final R (wR) is 0.063 (0.057) {w = 1/[σ2(F) + 0.0004F2]} for 3619 unique reflections measured at 295 K. The aryl phosphinate group bonded to the central phenyl ring comes close to one of the two glycidyl ether groups, the epoxide ring of which is ordered. The epoxide ring far from the aryl phosphinate group is disordered. The NMR chemical shifts of the protons of the glycidyl ether group close to the aryl phosphinate group are reduced by the 'ring-current effect'.
- Cho, Ching-Sheng,Liau, Wen-Bin,Chen, Leo-Wang
-
-
Read Online
- Preparation method of high-purity DOPO-HQ
-
The invention relates to a preparation method of high-purity 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide(DOPO-HQ). the preparation method comprises the following steps that activated carbon and atlapulgite are added into a 1,4-para benzoquinone solvent organic solvent, a decoloration reaction is conducted at 60-130 DEG C, and thus a treated 1,4-para benzoquinone solution is obtained; under the protective atmosphere, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is dissolved in the organic solvent, then the treated 1,4-para benzoquinone solution is added intothe organic solvent dropwise, reaction is conducted at 60-130 DEG C, and after complete reaction, a crude product is obtained; and the crude product is dissolved in the organic solvent, the activatedcarbon and the atlapulgite are added into the organic solvent, the crude product is subjected to a decoloration reaction at 60-130 DEG C, after complete reaction, the activated carbon and the atlapulgite are removed, cooling crystallization is conducted, and after a crystal is dried, the 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide is obtained. As for the DOPO-HQ prepared through the preparation method, the purity is 99.9% or above (HPLC), and the whiteness is 95 or above.
- -
-
Paragraph 0041-0057
(2019/11/13)
-
- A novel diol precursor for preparing flame-retardant polyurethane
-
The present invention relates to a novel diol precursor for manufacturing flame retardant polyurethane. The polyurethane manufactured by using the diol precursor for manufacturing the flame-retardant polyurethane of the present invention has excellent flame retardancy. In addition, after the thermoplastic flame retardant polyurethane is formed, a crosslinking reaction occurs by a double bond, resulting in thermosetting flame retardant polyurethane. As a result of cross-liked after processing, the thermosetting flame retardant polyurethane is excellent in durability as well as thermal stability.(AA) Step 1: crosslinkable flame retardant diol(BB) Step 2: flame-retardant polyurethane with double bonds(CC) Step 3: high durability flame-retardant polyurethane after crosslinking(DD) Durability(EE) Flame resistance(FF) All(GG) Phosphorus based flame retardant material(HH) Double bond(II) Urethane bindingCOPYRIGHT KIPO 2018
- -
-
Paragraph 0074; 0077; 0084; 0085
(2018/11/22)
-
- XANTHENE-CONTAINING OR THIOXANTHENE-CONTAINING PHOSPHINATED COMPOUNDS AND PREPARATION METHODS THEREOF
-
Xanthene-containing or thioxanthene-containing phosphinated compounds and preparation methods thereof are disclosed. The method includes reacting compounds (i) with compounds (ii) and compounds (iii) in the presence of an acid catalyst to synthesize compounds having the structure of formula (I).
- -
-
Page/Page column 10
(2018/04/07)
-
- DOPS-1,4 phenol and preparation method thereof
-
The invention discloses DOPS-1,4 phenol. The DOPS-1,4 phenol is characterized in that the formula is shown in the description. The DOPS-1,4 phenol is brown powdery solid, and the melting point ranges from 123 DEG C to 125 DEG C. A preparation operation method is simple, the yield is in the middle level, raw materials are wide in source, no severe pollution is produced, the repeatability is good, and mass production is easy.
- -
-
Paragraph 0017
(2016/10/10)
-
- Synthesis of flame-retardant phosphaphenanthrene derivatives with high phosphorus contents
-
Two novel types of phosphate derivatives of phosphaphenanthrene with a high phosphorus content were prepared by phosphorylation reaction between either 2-(6-oxido-6H-dibenzc,e1,2oxaphosphorin-6-yl)-methanol (ODOPM) or 2-(6-oxido-6H-dibenzc,e1,2.oxaphosphorin-6-yl)-1,4-benzenediol (ODOPB) and dialkyl phosphoryl chloride. The structures of all compounds were characterised by 1H NMR, 13C NMR, 31P NMR, Fourier transform infrared spectroscopy, and high-resolution mass spectrometry. The thermal stability of representative compounds was determined by thermal gravimetric analysis and differential scanning calorimetry. The results showed that the compounds have excellent resistance to oxidation, high thermal stability with an onset decomposition temperature above 200°C, and a high char yield over 25 %, owing to the high P content. The representative compound was added to conventional electrolytes of lithium-ion batteries as flame retardant additive, and the self-extinguishing time and ionic conductivity were measured. The result showed that the compounds have effective flame retardant properties.
- Zheng, Jinyun,Yu, Yujian,Zhang, Lulu,Zhen, Xiaomin,Zhao, Yufen
-
p. 1688 - 1692
(2015/01/09)
-
- Solubilities of (2,5-dihydroxyphenyl)diphenyl phosphine oxide in selected solvents
-
A phosphorus-containing flame retardant (2,5-dihydroxyphenyl)diphenyl phosphine oxide (HPO) was characterized by a differential scanning calorimeter (DSC), thermogravimetric analysis (TGA), elemental analysis, and nuclear magnetic resonance (1H NMR and 31P NMR). Using a static analytical method, the solubilities of HPO were measured in 12 solvents and correlated with an empirical equation. The estimated uncertainty of all of the solubility values on error analysis and repeated observations was within 2.0 %.
- Guo, Xiu-Zhi,Wang, Li-Sheng,Tian, Na-Na
-
body text
p. 1745 - 1749
(2011/07/31)
-
- Flame retardancy and thermal degradation mechanism of epoxy resin composites based on a DOPO substituted organophosphorus oligomer
-
A series of flame-retardant epoxy resins (EP) with different content of poly(DOPO substituted dihydroxyl phenyl pentaerythritol diphosphonate) (PFR) were prepared. The PFR was synthesized via the polycondensation between 10-(2,5-dihydroxyl phenyl)-9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO-BQ) and pentaerythritol diphosphonate dichloride (SPDPC). The structure of PFR was confirmed by Fourier transform infrared spectroscopy (FTIR) and 1H nuclear magnetic resonance (1H NMR). The flame retardancy and the thermal stability of the EP/PFR hybrids were investigated by limiting oxygen index (LOI) test and thermogravimetric analysis (TGA) in air. The results showed that the incorporation of PFR into EP can improve the thermal stability dramatically. The mechanical results demonstrated that PFR enhanced failure strain slightly accompanied by a decrease in tensile strength. The thermal oxidative degradation mechanisms of the EP/PFR hybrids were investigated by real time Fourier transform infrared spectra (RTFTIR) and direct pyrolysis/mass (DP-MS) analysis. X-ray photoelectron spectroscopy (XPS) was used to explore chemical components of the residual char of EP and EP/PFR hybrid. DP-MS analysis showed that the degradation process of EP/PFR hybrid was divided into two characteristic temperature regions, attributed to the decomposition of phosphate and aromatic structure.
- Wang, Xin,Hu, Yuan,Song, Lei,Xing, Weiyi,Lu, Hongdian,Lv, Pin,Jie, Ganxin
-
experimental part
p. 2435 - 2445
(2011/10/07)
-
- Palladium-catalyzed arylation of 9,10-Dihydro-9-oxa-10-phosphaphenanthrene- 10-oxide (DOPO) with halogen-substituted phenols
-
Phenol functionalized 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) derivatives are synthesized via palladium-catalyzed arylation of DOPO with halogen-substituted phenols. 2-,3-, and 4-Substituted halogen phenols are successfully applied to th
- Yang, Liancheng,Xu, Longhe,Tao, Zaizhou
-
experimental part
p. 3175 - 3181
(2010/05/19)
-
