CN1673260A - Modifier and its prepn process - Google Patents
Modifier and its prepn process Download PDFInfo
- Publication number
- CN1673260A CN1673260A CN 200410014390 CN200410014390A CN1673260A CN 1673260 A CN1673260 A CN 1673260A CN 200410014390 CN200410014390 CN 200410014390 CN 200410014390 A CN200410014390 A CN 200410014390A CN 1673260 A CN1673260 A CN 1673260A
- Authority
- CN
- China
- Prior art keywords
- acid
- modification agent
- polyol ester
- whitfield
- ointment
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000003607 modifier Substances 0.000 title abstract 4
- -1 borate ester Chemical class 0.000 claims abstract description 37
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 34
- 230000004048 modification Effects 0.000 claims description 33
- 238000012986 modification Methods 0.000 claims description 33
- 229920005862 polyol Polymers 0.000 claims description 30
- 239000002253 acid Substances 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 239000003054 catalyst Substances 0.000 claims description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 9
- 238000005516 engineering process Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 8
- 235000021355 Stearic acid Nutrition 0.000 claims description 8
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 8
- 239000004327 boric acid Substances 0.000 claims description 8
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 8
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 8
- 239000008117 stearic acid Substances 0.000 claims description 8
- 230000002378 acidificating effect Effects 0.000 claims description 6
- CUBCNYWQJHBXIY-UHFFFAOYSA-N benzoic acid;2-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=CC=C1.OC(=O)C1=CC=CC=C1O CUBCNYWQJHBXIY-UHFFFAOYSA-N 0.000 claims description 6
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 6
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- 150000007524 organic acids Chemical class 0.000 claims description 6
- USYAMXSCYLGBPT-UHFFFAOYSA-L 3-carboxy-3-hydroxypentanedioate;tin(2+) Chemical compound [Sn+2].OC(=O)CC(O)(C([O-])=O)CC([O-])=O USYAMXSCYLGBPT-UHFFFAOYSA-L 0.000 claims description 4
- 239000005711 Benzoic acid Substances 0.000 claims description 4
- 235000010233 benzoic acid Nutrition 0.000 claims description 4
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 4
- 235000011187 glycerol Nutrition 0.000 claims description 4
- MEIRRNXMZYDVDW-MQQKCMAXSA-N (2E,4E)-2,4-hexadien-1-ol Chemical compound C\C=C\C=C\CO MEIRRNXMZYDVDW-MQQKCMAXSA-N 0.000 claims description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 3
- 239000005639 Lauric acid Substances 0.000 claims description 3
- 239000005642 Oleic acid Substances 0.000 claims description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 3
- 235000021314 Palmitic acid Nutrition 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 3
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 claims description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 3
- 229940098695 palmitic acid Drugs 0.000 claims description 3
- 229940059574 pentaerithrityl Drugs 0.000 claims description 3
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N propylene glycol Substances CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 2
- 235000021313 oleic acid Nutrition 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 2
- 239000007822 coupling agent Substances 0.000 abstract description 13
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 229920000620 organic polymer Polymers 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 230000000051 modifying effect Effects 0.000 abstract description 2
- 150000005846 sugar alcohols Polymers 0.000 abstract 4
- 229960001860 salicylate Drugs 0.000 abstract 2
- 239000004605 External Lubricant Substances 0.000 abstract 1
- 239000004610 Internal Lubricant Substances 0.000 abstract 1
- 230000003712 anti-aging effect Effects 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 238000003754 machining Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 13
- 239000004800 polyvinyl chloride Substances 0.000 description 13
- 235000012204 lemonade/lime carbonate Nutrition 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000012764 mineral filler Substances 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 239000012752 auxiliary agent Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000004743 Polypropylene Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- 239000004709 Chlorinated polyethylene Substances 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 229910052918 calcium silicate Inorganic materials 0.000 description 2
- 235000012241 calcium silicate Nutrition 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000009499 grossing Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 229910004762 CaSiO Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000006057 Non-nutritive feed additive Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Images
Abstract
The present invention discloses one kind of modifier and its preparation process. The modifier is one kind of compound material of polyhydric alcohol borate ester and polyhydric alcohol salicylate ester prepared through heating polyhydric alcohol borate ester and polyhydric alcohol salicylate ester in certain ratio to react. The modifier has functions of being used as coupling agent, dispersant, internal and external lubricant, etc. and has unique organic polymer modifying effects, including promoting plasticization, raising dispersivity, improving antiageing and machining performance, realizing high stuffing, etc.
Description
Technical field
The invention belongs to organic polymer composite auxiliary agent field, particularly relate to a kind of modification agent and preparation method thereof.
Background technology
When organic polymer composite goods such as production plastics, need usually to add some mineral fillers at present (as CaCO
3, CaSiO
3), generally carry out surface treatment with auxiliary agents such as stearic acid, coupling agents, can improve the product section performance on the one hand, also can reduce production costs on the other hand, but general coupling agent color and luster is dark, processing characteristics, ageing resistance are undesirable, it is more obvious when especially the mineral filler height is filled, objectively limited the usage quantity of mineral filler, the auxiliary agent function singleness of Shi Yonging in the market, and kind is few, quality is low, so need on the market a kind ofly can realize that mineral filler is high and fill, reduce production costs the auxiliary agent of can improve quality product again, enhancing product performance.
Summary of the invention
The objective of the invention is to overcome above-mentioned shortcoming, a kind of compound modification agent that promotes to plastify, improve dispersion, improves performance is provided.
Another object of the present invention provides the preparation method of above-mentioned modification agent.
Purpose of the present invention can realize by following measure:
A kind of modification agent comprises the prescription of following weight percent:
Acid polyol ester 20%-70%, Whitfield's ointment polyol ester 30%-80%.
Described modification agent, wherein acid polyol ester is formed by boric acid and polyvalent alcohol and organic acid chemical combination.
Described modification agent, wherein polyvalent alcohol can be glycerine, ethylene glycol, glycol ether, 1.2-propylene glycol, tetramethylolmethane, sorbyl alcohol.
Described modification agent, wherein organic acid can be lauric acid, oleic acid, stearic acid, Palmiticacid, vinylformic acid.
The preparation technology of described modification agent comprises the following step:
A. boric acid is mixed with polyvalent alcohol and organic acid, add non-acidic catalyst, heated and stirred, temperature are controlled at 180-210 ℃, react 3-5 hour, and reaction is finished, and filter, and get acid polyol ester, and be standby;
B. Whitfield's ointment is mixed with polyvalent alcohol, add non-acidic catalyst, heated and stirred, temperature are controlled at 180-215 ℃, react 4-6 hour, and reaction is finished, and filter, and get the Whitfield's ointment polyol ester, and be standby;
C. by prescription acid polyol ester is mixed with the Whitfield's ointment polyol ester, be heated to 130-150 ℃, reacted 40-60 minute, reaction is finished, and filters.
The preparation technology of described modification agent, wherein non-acidic catalyst is organotin catalysts or titanate catalyst.
The preparation technology of described modification agent, wherein organotin catalysts can be the inferior tin, benzoic acid stannous of stannous citrate, formic acid.
The preparation technology of described modification agent, wherein titanate catalyst can be tetrabutyl titanate, titanium isopropylate.
Advantage of the present invention:
Modification agent of the present invention has multiple functions such as coupling agent, dispersion agent, inside and outside lubricant agent, goods such as plastics had unique modifying function, can promote plasticizing, improve to disperse, improve aging and processing characteristics, have coupling enhancing and an effect on thermal simultaneously, improve the physical and mechanical properties and the surface luster of goods, and can realize the high filling of mineral filler, reduce production costs.
The present invention also can use in rubber, paint field.
One, modification agent of the present invention is at PVC/CaCO
3Infill system is to improving the experiment of PVC product performance
Press the listed formula for a product of table 1 and make two kinds of products of A, B, modification agent of the present invention is pressed embodiment 1 preparation in the prescription, and the performance test results of A, two kinds of products of B sees Table 2.
Table 1 reference product prescription (unit: weight part)
| Formula for a product | The A product | The B product |
| PVC(SG-5) | 100 | ?100 |
| Acrylate processing aid (ACR401) | 2 | ?2 |
| Chlorinatedpolyethylene (CPE) | 8.5 | ?8 |
| Titanium dioxide (rutile) | 4.5 | ?4.5 |
| Stablizer (FWR-XC-B) * | 4.5 | ?4.5 |
| Light calcium carbonate | 10 | ?25 |
| Modification agent of the present invention | 0.4 | |
| Pigment | In right amount | In right amount |
*: the FWR-XC-B stablizer is that Nanjing Xiehe Chemistry Co., Ltd. produces.
Table 2 performance comparison (pressing the GB8814-98 standard testing)
| Test item | Technical indicator | The A product | The B product | Individual event is judged |
| Hardness (HRR) | ≥85 | ?90 | ?102 | Qualified |
| Tensile yield strength (MPa) | ≥37 | ?40 | ?41 | Qualified |
| Elongation at break (%) | ≥100 | ?143 | ?159 | Qualified |
| Bending elastic modulus (MPa) | ≥1960 | ?2160 | ?2250 | Qualified |
| Low temperature drop impact (individual) | Number≤1 breaks | ?1 | ?0 | Qualified |
| Qualified Vicat softening point (℃) | ≥83 | ?85 | ?86 | Qualified |
| Heating back state | No bubble, slight crack, pit | No bubble, slight crack, pit | Qualified | |
| Heating back size changing rate (%) | ±2.5 | ?-2.0 | ?1.9 | Qualified |
| Hydrogen index (HI) (%) | ≥38 | ?≥40 | ?41 | Qualified |
| High low temperature size changing rate (%) | ±0.2 | ?-0.15 | ?-0.1 | Qualified |
| Shock strength (kJ/m 2) | ≥40(23±2℃) | ?53 | ?57 | Qualified |
| Shock strength (kJ/m 2) | ≥15(-10±1℃) | ?51 | ?53 | Qualified |
| Sinuousness (mm) | ≤2.0 | ?≤1.0 | ?0.5 | Qualified |
| Outward appearance | Surface smoothing, flawless, impurity etc. | Surface smoothing, flawless, impurity etc. | Qualified | |
| Fillet weld strength (N) | ≥3000 | ?5460 | ?5150 | Qualified |
Conclusion: adopt the PVC product physical and mechanical properties of modification agent of the present invention to be significantly improved, can realize that the increment of light calcium carbonate is filled simultaneously, reduce production costs.
Two, modification agent of the present invention and coupling agent are used for polyacrylic mechanical property relatively
Modification agent of the present invention and coupling agent show relatively that to polyacrylic mechanical property modification agent of the present invention can obviously improve polyacrylic mechanical property, and effect is good than coupling agent, the results are shown in Table 3.
Table 3 the present invention and coupling agent are used for polyacrylic mechanical property relatively
| Prescription (wt%) | Tensile strength (MbPa) | Notched Izod impact strength (kJ/m 2) | |
| ????25℃ | ????-30℃ | ||
| Polypropylene | ????31.9 | ????4.6 | ????2.3 |
| Polypropylene (70%)+titanate coupling agent NDE-101 modified grammite (30%) | ????25.8 | ????8.5 | ????6.0 |
| Polypropylene (70%)+modification agent modified grammite of the present invention (30%) | ????27.3 | ????11.5 | ????8.1 |
Three, the present invention is to the deployment conditions influence of lime carbonate in the polyvinyl chloride
By lime carbonate deployment conditions electromicroscopic photograph in polyvinyl chloride of handling with modification agent of the present invention, stearic acid, titanate coupling agent is respectively compared, as can be seen, the lime carbonate of handling through stearic acid disperses inhomogeneous in polyvinyl chloride, granular size differs, and obvious agglomeration (see figure 1) is arranged; The lime carbonate of handling through titanate coupling agent disperses more even in polyvinyl chloride, and particle is bigger, and the agglomeration (see figure 2) is arranged; The lime carbonate of handling through modification agent of the present invention is uniformly dispersed in polyvinyl chloride, particle exquisiteness, no agglomeration (see figure 3).By knowing as can be known, modification agent of the present invention is to the effect of having clear improvement of polyvinyl chloride product performance, and is more obvious than stearic acid, titanate coupling agent effect.
Description of drawings
Fig. 1 is the electromicroscopic photograph of lime carbonate deployment conditions in polyvinyl chloride of handling with stearic acid.
Fig. 2 is the electromicroscopic photograph of lime carbonate deployment conditions in polyvinyl chloride of handling with titanate coupling agent.
Fig. 3 is the electromicroscopic photograph of lime carbonate deployment conditions in polyvinyl chloride of handling with modification agent of the present invention.
Embodiment
Following examples are for further illustrating the present invention, but do not limit the present invention.
Embodiment 1
Boric acid 50g is mixed with ethylene glycol 110g and oleic acid 200g, add catalyzer metatitanic acid four butyl esters, heated and stirred, temperature are controlled at 210 ℃, react 4 hours, and reaction is finished, and filters, and promptly gets acid polyol ester, and is standby; Whitfield's ointment 200g is mixed with glycol ether 165g, add catalyzer metatitanic acid four butyl esters, heated and stirred, temperature are controlled at 200 ℃, react 5 hours, and reaction is finished, and filters, and promptly gets the Whitfield's ointment polyol ester, and is standby; Get acid polyol ester 600g by prescription and mix with Whitfield's ointment polyol ester 400g, be heated to 150 ℃, reacted 40 minutes, reaction is finished, and filters promptly.
Embodiment 2
Boric acid 50g is mixed with sorbyl alcohol 310g and stearic acid 230g, add the catalyzer stannous citrate, heated and stirred, temperature are controlled at 195 ℃, react 4 hours, and reaction is finished, and filter, and promptly get acid polyol ester, and be standby; Whitfield's ointment 200g is mixed with glycerine 150g, add the catalyzer stannous citrate, heated and stirred, temperature are controlled at 210 ℃, react 4 hours, and reaction is finished, and filter, and promptly get the Whitfield's ointment polyol ester, and be standby; Get acid polyol ester 500g by prescription and mix with Whitfield's ointment polyol ester 500g, be heated to 130 ℃, reacted 60 minutes, reaction is finished, and filters promptly.
Embodiment 3
Boric acid 50g is mixed with tetramethylolmethane 235g and Palmiticacid 210g, and the adding catalyzer is benzoic acid stannous, and heated and stirred, temperature are controlled at 205 ℃, react 4 hours, and reaction is finished, and filters, and promptly gets acid polyol ester, and is standby; Whitfield's ointment 200g is mixed with 1.2-propylene glycol 125g, add the inferior tin of catalyzer formic acid, heated and stirred, temperature are controlled at 190 ℃, react 4 hours, and reaction is finished, and filters, and promptly gets the Whitfield's ointment polyol ester, and is standby; Get acid polyol ester 200g by prescription and mix with Whitfield's ointment polyol ester 800g, be heated to 140 ℃, reacted 45 minutes, reaction is finished, and filters promptly.
Embodiment 4
Boric acid 50g is mixed with glycol ether 180g and lauric acid 165g, and the adding catalyzer is benzoic acid stannous, and heated and stirred, temperature are controlled at 200 ℃, react 4 hours, and reaction is finished, and filters, and promptly gets acid polyol ester, and is standby; Whitfield's ointment 200g is mixed with glycerine 150g, add catalyzer metatitanic acid four isopropyl esters, heated and stirred, temperature are controlled at 210 ℃, react 4 hours, and reaction is finished, and filters, and promptly gets the Whitfield's ointment polyol ester, and is standby; Get acid polyol ester 700g by prescription and mix with Whitfield's ointment polyol ester 300g, be heated to 150 ℃, reacted 40 minutes, reaction is finished, and filters promptly.
Claims (8)
1, a kind of modification agent is characterized in that comprising the prescription of following weight percent:
Acid polyol ester 20%-70%, Whitfield's ointment polyol ester 30%-80%.
2, modification agent according to claim 1 is characterized in that acid polyol ester is wherein formed by boric acid and polyvalent alcohol and organic acid chemical combination.
3, modification agent according to claim 2 is characterized in that polyvalent alcohol wherein can be glycerine, ethylene glycol, glycol ether, 1.2-propylene glycol, tetramethylolmethane, sorbyl alcohol.
4, modification agent according to claim 2 is characterized in that organic acid wherein can be lauric acid, oleic acid, stearic acid, Palmiticacid, vinylformic acid.
5, a kind of preparation technology of modification agent is characterized in that comprising the following step:
A. boric acid is mixed with polyvalent alcohol and organic acid, add non-acidic catalyst, heated and stirred, temperature are controlled at 180-210 ℃, react 3-5 hour, and reaction is finished, and filter, and get acid polyol ester, and be standby;
B. Whitfield's ointment is mixed with polyvalent alcohol, add non-acidic catalyst, heated and stirred, temperature are controlled at 180-215 ℃, react 4-6 hour, and reaction is finished, and filter, and get the Whitfield's ointment polyol ester, and be standby;
C. by prescription acid polyol ester is mixed with the Whitfield's ointment polyol ester, be heated to 130-150 ℃, reacted 40-60 minute, reaction is finished, and filters.
6, the preparation technology of modification agent according to claim 5 is characterized in that non-acidic catalyst is organotin catalysts or titanate catalyst.
7, the preparation technology of modification agent according to claim 6 is characterized in that organotin catalysts can be the inferior tin, benzoic acid stannous of stannous citrate, formic acid.
8, the preparation technology of modification agent according to claim 6 is characterized in that titanate catalyst can be tetrabutyl titanate, titanium isopropylate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100143904A CN1304472C (en) | 2004-03-23 | 2004-03-23 | Modifier and its prepn process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100143904A CN1304472C (en) | 2004-03-23 | 2004-03-23 | Modifier and its prepn process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1673260A true CN1673260A (en) | 2005-09-28 |
| CN1304472C CN1304472C (en) | 2007-03-14 |
Family
ID=35046049
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100143904A Expired - Fee Related CN1304472C (en) | 2004-03-23 | 2004-03-23 | Modifier and its prepn process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1304472C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701986A (en) * | 2012-06-19 | 2012-10-03 | 芮立 | Method for preparing antioxidant for plastic or rubber processing |
| CN102702244A (en) * | 2012-06-19 | 2012-10-03 | 芮立 | Method for preparing additive for surface activation of plastic or rubber filler |
| CN104910413A (en) * | 2015-05-28 | 2015-09-16 | 青阳县恒源化工原料有限责任公司 | High-plasticity heavy active calcium carbonate |
| CN109422858A (en) * | 2017-08-19 | 2019-03-05 | 中国铁道科学研究院铁道建筑研究所 | A kind of polyalcohol being grafted UV absorption agent molecule |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456969B (en) * | 2008-12-29 | 2011-11-09 | 南京协和化学有限公司 | Functional calcium carbonate and method for producing the same |
| US8943716B2 (en) | 2011-10-10 | 2015-02-03 | Caterpillar Inc. | Implement tooth assembly with tip and adapter |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5153029A (en) * | 1989-08-11 | 1992-10-06 | Eastman Kodak Company | Solid-form additive systems dispersible in aqueous media, methods for the preparation and application thereof to polymeric particles |
-
2004
- 2004-03-23 CN CNB2004100143904A patent/CN1304472C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701986A (en) * | 2012-06-19 | 2012-10-03 | 芮立 | Method for preparing antioxidant for plastic or rubber processing |
| CN102702244A (en) * | 2012-06-19 | 2012-10-03 | 芮立 | Method for preparing additive for surface activation of plastic or rubber filler |
| CN102701986B (en) * | 2012-06-19 | 2014-01-29 | 芮立 | Method for preparing antioxidant for plastic or rubber processing |
| CN102702244B (en) * | 2012-06-19 | 2015-11-18 | 芮立 | Plastics or the rubber filler preparation method of surface activation process additive |
| CN104910413A (en) * | 2015-05-28 | 2015-09-16 | 青阳县恒源化工原料有限责任公司 | High-plasticity heavy active calcium carbonate |
| CN109422858A (en) * | 2017-08-19 | 2019-03-05 | 中国铁道科学研究院铁道建筑研究所 | A kind of polyalcohol being grafted UV absorption agent molecule |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1304472C (en) | 2007-03-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101678049B1 (en) | Thermoplastic elastomer composition and use thereof | |
| CN101880429A (en) | High-tenacity heat-resisting ageing-resisting chlorinated polyvinyl chloride alloy material and preparation method thereof | |
| CN1304472C (en) | Modifier and its prepn process | |
| CN101289573A (en) | Method for preparing novel alloy based on chlorinated polyethylene and thermoplastic polyurethane | |
| CN101635385A (en) | PVC profile outer cover used in base station antenna and preparation method thereof | |
| CN1276393A (en) | Composition used for fire resistant industrial wall slab and its production technology | |
| CN102807708B (en) | Aedelforsite powder modified filling master batch applied to flat silks and method for producing flat silks | |
| CN1233725C (en) | Soft polyvinyl chloride composition and its preparation method | |
| CN1596281A (en) | Molding compositions having improved properties | |
| CN1908060A (en) | Preparation method for flame-proof acrylonitrile-styrene copolymerized resin/acrylonitrile-chlorided polyethylene-styrene copolymerized resinplastic alloy | |
| CN100335546C (en) | Rubber composition for sidewall and inflatable tyre made from it | |
| CN106496801A (en) | PP composite material preparation method and its PP composite material of preparation | |
| DE102010031892B4 (en) | Fiber-reinforced composites, processes for their preparation and their use | |
| CN1908059A (en) | Preparation method for acrylonitrile-styrene copolymerized resin/acrylonitrile-chlorided polyethylene-styrene copolymerized resin_plastic alloy | |
| CN1276021C (en) | Polyvinyl chloride function modifier and its prepn process | |
| CN1105744C (en) | Water-proof coiled material of chlorated polyethylene modified by superhigh-molecular polyvinyl chloride | |
| CN1597753A (en) | Nitrile polymer mixer used for magnetic sealing | |
| CN1664004A (en) | Polyester/unidimensional nano silicate composite materials and method for preparing same | |
| CN1208386C (en) | Specific meterial for modified polypropylene TV housing and production method thereof | |
| CN1334842A (en) | Mouding substances based poly-C 2-6-alkylene terephthalates | |
| CN1732227A (en) | Thermoplastic elastomer resin | |
| DE602005004854T2 (en) | Crosslinking of Carboxylated Nitrile Polymers with Organofunctional Silanes: A Curable Softening Composition | |
| CN1546570A (en) | Composite material of fibrous nanometer clay and high viscosity polyamide | |
| KR101212456B1 (en) | Resin pipe having improved impact resistance | |
| CN1408768A (en) | Formulation of full environment protection thermoplastic polyurethane (TPU) film and its calendering production method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20200909 Address after: No.90-98, Fangshui Road, Nanjing Chemical Industrial Park, Nanjing, Jiangsu Province, 210024 Patentee after: NANJING CONCORD FERTILIZER CHEMISTRY LTD. Address before: 210024 No. 228, Guangzhou Road, Gulou District, Jiangsu, Nanjing Patentee before: Nanjing Xiehe Chemical Co.,Ltd. |
|
| TR01 | Transfer of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20070314 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |