CN104650325A - Novel polyester polyol and preparation method thereof - Google Patents
Novel polyester polyol and preparation method thereof Download PDFInfo
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- CN104650325A CN104650325A CN201510058927.5A CN201510058927A CN104650325A CN 104650325 A CN104650325 A CN 104650325A CN 201510058927 A CN201510058927 A CN 201510058927A CN 104650325 A CN104650325 A CN 104650325A
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Abstract
The invention discloses a novel polyester polyol and a preparation method thereof. The preparation method comprises the following steps: (1) at the room temperature, preparing a blend from dibasic acid dimethyl ester or dibasic acid diethyl ester, dibasic acid, and pentaerythritol, wherein the molar ratio of dibasic acid dimethyl ester or dibasic acid diethyl ester to dibasic acid is 1:1 to 8:1, and the molar ratio of dibasic acid dimethyl ester or both dibasic acid diethyl ester and dibasic acid to pentaerythritol is 1:1 to 1:3; adding the blend into a reaction kettle which is provided with an electric stirrer, an electric heater, a reflux condenser and a temperature measuring system, and adding a catalyst which is 0.3%-3% (in fraction by mass) of the blend; (2) gradually heating the reaction kettle to 200-240 DEG C, and reacting for 4-6 hours to obtain the novel polyester polyol. The preparation for the novel novel polyester polyol is relatively low in cost and relatively low in energy consumption; solvents of acetone and the like are not needed to be additionally added when obtained polyester polyol reacts with diisocyanate to synthesize polyurethane, so that the polyurethane is relatively quick to mould and relatively environment-friendly in synthesis process.
Description
Technical field
The present invention relates to polyester polyol and preparation method thereof, particularly relate to a kind of new polyester polyvalent alcohol and preparation method thereof.
Background technology
Polyester polyol is the novel polymer polyatomic alcohol of a class, and its molecular backbone chain is made up of carboxylic ester group, and end group is hydroxyl, can as the base mateiral of tensio-active agent or polyurethane material.Be that polyurethane material prepared by raw material has higher intensity, excellent wear resisting property, oil-proofness, weathering resistance and anti-hydrolytic performance with polyester polyol, also there is good biodegradability, may be used for producing polyurethane elastomer, coating, tackiness agent, foam materials etc., therefore polyester polyol is as the novel high performance polyurethane starting material of a class, receives the extensive welcome of manufacturer.But current polyester polyol is with the process of di-isocyanate reaction synthesis of polyurethane, in order to reduce the viscosity of reactant in building-up process, avoid occurring rod climbing phenomenon, enable reactant chain extension further simultaneously, reach required molecular weight, all need additionally to add acetone equal solvent to assist, and need be cross-linked through preheating or external force, just can make polyurethane moulded, and after completion of the reaction, also need to set up step in addition to reclaim acetone equal solvent, cause with cost during existing polyester polyol synthesis of polyurethane is higher and technique is comparatively complicated.
Summary of the invention
The object of the invention is in order to solve the existing polyester polyol that exists in prior art all need additionally to add solvent when synthesis of polyurethane and need through long-time preheating or external force is crosslinked could the defect such as synthesis of polyurethane, provide a kind of new polyester polyvalent alcohol and preparation method thereof.
In order to solve the problems of the technologies described above, the present invention is achieved through the following technical solutions:
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 1:1 ~ 8:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:1 ~ 1:3 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 0.3% ~ 3% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C ~ 240 DEG C, react 4 hours ~ 6 hours, namely obtain a kind of new polyester polyvalent alcohol.
The new polyester polyvalent alcohol prepared by the present invention, with di-isocyanate reaction synthesis of polyurethane process in without the need to adding acetone equal solvent in addition, and can not rod climbing phenomenon be there is, eliminate the step reclaiming acetone equal solvent simultaneously, reduce the cost in synthesis of polyurethane process and decrease processing step, accelerating the synthesis of urethane, and the cost of material that the present invention uses when preparing polyester polyol is cheap, in preparation process, required energy consumption is low, is convenient to large-scale promotion and uses.
As preferably, the preparation method of a kind of new polyester polyvalent alcohol described above, in described step (1), described dibasic acid dimethyl ester is any one in dimethyl sebacate, dimethyl succinate, dimethyl adipate or the mixtures more than any two, and described binary acids diethyl esters is any one in ethyl sebacate, diethyl succinate, diethylene adipate or the mixtures more than any two.Select above material to carry out transesterification reaction, whole reaction process can be made more easily to carry out, improve transformation efficiency.
As preferably, the preparation method of a kind of new polyester polyvalent alcohol described above, the diprotic acid in described step (1) is any one in sebacic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, dimeracid or the mixtures more than any two.Above material is comparatively conventional, is easy to obtain, and transformation efficiency is higher.
As preferably, the preparation method of a kind of new polyester polyvalent alcohol described above, described step can also add carbon long-chain in (1), the massfraction of described carbon long-chain is 1% ~ 40% of blend, and described carbon long-chain is any one in Viscotrol C, hydrogenated castor oil, polyoxyethylene glycol, polypropylene glycol or the mixtures more than any two.By block carbon long-chain, the crystal property of the polyester polyol obtained can be changed, reduce fusing point.
As preferably, the preparation method of a kind of new polyester polyvalent alcohol described above, the catalyzer in described step (1) is any one or any two above mixtures in tetrabutyl titanate, dibutyl tin laurate, tin protochloride.Accelerated reaction can carry out, improve the yield of polyester polyol.
As preferably, the preparation method of a kind of new polyester polyvalent alcohol described above, dibasic acid dimethyl ester in described step (1) or the mol ratio of binary acids diethyl esters and diprotic acid are 1:1 ~ 4:1, and dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid are 1:1 ~ 1:1.5 with the mol ratio of tetramethylolmethane.The structure of the polyester polyol obtained can be made to become more tight.
As preferably, the preparation method of a kind of new polyester polyvalent alcohol described above, the massfraction that the catalyzer in described step (1) accounts for blend is 0.3% ~ 1%.Can the carrying out of accelerated reaction better within the scope of this, improve transformation efficiency.
A kind of new polyester polyvalent alcohol, is obtained by the preparation method of any one new polyester polyvalent alcohol above-mentioned.
Beneficial effect of the present invention is: the cost of material that the present invention uses when preparing new polyester polyvalent alcohol is cheap, required energy consumption is low in preparation process, significantly can reduce the production cost of this new polyester polyvalent alcohol, and the new polyester polyol quality obtained is higher, without the need to adding acetone equal solvent in addition when the new polyester polyvalent alcohol prepared with the present invention and di-isocyanate reaction synthesis of polyurethane, also without the need to reclaiming acetone equal solvent, and the crosslinked step of preheating or external force can be removed from, make polyurethane moulded faster and building-up process more environmental protection.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but they are not limitations of the present invention:
embodiment 1
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 1:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:1 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 0.3% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 2
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 8:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:1 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 0.3% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 3
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 4:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:1 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 0.3% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 4
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 1:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:3 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 0.3% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 5
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 8:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:3 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 0.3% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 6
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 4:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:3 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 0.3% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 7
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 1:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:1.5 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 0.3% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 8
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 8:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:1.5 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 0.3% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 9
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 4:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:1.5 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 0.3% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 10
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 1:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:1 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 3% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 11
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 8:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:1 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 3% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 12
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 4:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:1 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 3% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 13
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 1:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:3 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 3% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 14
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 8:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:3 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 3% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 15
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 4:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:3 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 3% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 16
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 1:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:1.5 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 3% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 17
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 8:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:1.5 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 3% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 18
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 4:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:1.5 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 3% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 19
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 1:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:1 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 1% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 20
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 8:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:1 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 1% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 21
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 4:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:1 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 1% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 22
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 1:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:3 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 1% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 23
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 8:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:3 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 1% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 24
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 4:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:3 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 1% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 25
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 1:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:1.5 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 1% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 26
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 8:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:1.5 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 1% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 27
A preparation method for new polyester polyvalent alcohol, comprises the following steps:
(1) at room temperature, be 4:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:1.5 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 1% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C, react 4 hours, namely obtain a kind of new polyester polyvalent alcohol.
The wherein preferred dimethyl sebacate of dibasic acid dimethyl ester, dimethyl succinate, any one in dimethyl adipate or the mixtures more than any two, the preferred ethyl sebacate of described binary acids diethyl esters, diethyl succinate, any one in diethylene adipate or the mixtures more than any two, the preferred sebacic acid of diprotic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, any one in dimeracid or the mixtures more than any two, the preferred tetrabutyl titanate of catalyzer, dibutyl tin laurate, any one in tin protochloride or the mixtures more than any two.
embodiment 28
In described step (2), progressively heated up by reactor, rise to 240 DEG C, react 4 hours, other step is with embodiment 1 to 27.
embodiment 29
In described step (2), progressively heated up by reactor, rise to 220 DEG C, react 4 hours, other step is with embodiment 1 to 27.
embodiment 30
In described step (2), progressively heated up by reactor, rise to 200 DEG C, react 6 hours, other step is with embodiment 1 to 27.
embodiment 31
In described step (2), progressively heated up by reactor, rise to 240 DEG C, react 6 hours, other step is with embodiment 1 to 27.
embodiment 32
In described step (2), progressively heated up by reactor, rise to 220 DEG C, react 6 hours, other step is with embodiment 1 to 27.
embodiment 33
In described step (2), progressively heated up by reactor, rise to 200 DEG C, react 5 hours, other step is with embodiment 1 to 27.
embodiment 34
In described step (2), progressively heated up by reactor, rise to 240 DEG C, react 5 hours, other step is with embodiment 1 to 27.
embodiment 35
In described step (2), progressively heated up by reactor, rise to 220 DEG C, react 5 hours, other step is with embodiment 1 to 27.
embodiment 36
Described step can also add carbon long-chain in (1), and the massfraction of described carbon long-chain is 1% of blend, and described carbon long-chain is any one in Viscotrol C, hydrogenated castor oil, polyoxyethylene glycol, polypropylene glycol or the mixtures more than any two.Other step is with embodiment 1 to 35.
embodiment 37
Described step can also add carbon long-chain in (1), and the massfraction of described carbon long-chain is 40% of blend, and described carbon long-chain is any one in Viscotrol C, hydrogenated castor oil, polyoxyethylene glycol, polypropylene glycol or the mixtures more than any two.Other step is with embodiment 1 to 35.
embodiment 38
Described step can also add carbon long-chain in (1), and the massfraction of described carbon long-chain is 20% of blend, and described carbon long-chain is any one in Viscotrol C, hydrogenated castor oil, polyoxyethylene glycol, polypropylene glycol or the mixtures more than any two.Other step is with embodiment 1 to 35.
embodiment 39
Get the new polyester polyvalent alcohol that any embodiment in the 100g embodiment of the present invention 1 ~ 38 prepares, measure its hydroxyl value, make itself and vulcabond at 60 DEG C, react 2 minutes under the condition of equivalence ratio=0.95 of NCO/OH, can urethane be obtained.
embodiment 40
Get the new polyester polyvalent alcohol that any embodiment in the 100g embodiment of the present invention 1 ~ 38 prepares, measure its hydroxyl value, make itself and vulcabond at 60 DEG C, react 6 minutes under the condition of equivalence ratio=2 of NCO/OH, can urethane be obtained.
embodiment 41
Get the new polyester polyvalent alcohol that any embodiment in the 100g embodiment of the present invention 1 ~ 38 prepares, measure its hydroxyl value, make itself and vulcabond at 60 DEG C, react 4 minutes under the condition of equivalence ratio=1.5 of NCO/OH, can urethane be obtained.
In a word, the foregoing is only preferred embodiment of the present invention, all equalizations done according to the scope of the present patent application patent change and modify, and all should belong to covering scope of the present invention.
Claims (8)
1. a preparation method for new polyester polyvalent alcohol, is characterized in that: comprise the following steps:
(1) at room temperature, be 1:1 ~ 8:1 by the mol ratio of dibasic acid dimethyl ester or binary acids diethyl esters and diprotic acid, the proportions being 1:1 ~ 1:3 with the mol ratio of tetramethylolmethane by dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid becomes blend to drop in the reactor that electric mixer, electric heater, reflux exchanger, temp measuring system are housed, and adds the catalyzer that massfraction is 0.3% ~ 3% of blend;
(2) reactor is progressively heated up, rise to 200 DEG C ~ 240 DEG C, react 4 hours ~ 6 hours, namely obtain a kind of new polyester polyvalent alcohol.
2. according to the preparation method of a kind of new polyester polyvalent alcohol described in claim 1, it is characterized in that: in described step (1), described dibasic acid dimethyl ester is any one in dimethyl sebacate, dimethyl succinate, dimethyl adipate or the mixtures more than any two, and described binary acids diethyl esters is any one in ethyl sebacate, diethyl succinate, diethylene adipate or the mixtures more than any two.
3. according to the preparation method of a kind of new polyester polyvalent alcohol described in claim 1, it is characterized in that: the diprotic acid in described step (1) is any one in sebacic acid, hexanodioic acid, succinic acid, terephthalic acid, tartrate, fumaric acid, dimeracid or the mixtures more than any two.
4. according to the preparation method of a kind of new polyester polyvalent alcohol described in claim 1, it is characterized in that: described step can also add carbon long-chain in (1), the massfraction of described carbon long-chain is 1% ~ 40% of blend, and described carbon long-chain is any one in Viscotrol C, hydrogenated castor oil, polyoxyethylene glycol, polypropylene glycol or the mixtures more than any two.
5. according to the preparation method of a kind of new polyester polyvalent alcohol described in claim 1, it is characterized in that: the catalyzer in described step (1) is any one in tetrabutyl titanate, dibutyl tin laurate, tin protochloride or the mixtures more than any two.
6. according to the preparation method of a kind of new polyester polyvalent alcohol described in claim 1, it is characterized in that: the dibasic acid dimethyl ester in described step (1) or the mol ratio of binary acids diethyl esters and diprotic acid are 1:1 ~ 4:1, dibasic acid dimethyl ester or binary acids diethyl esters, both diprotic acid are 1:1 ~ 1:1.5 with the mol ratio of tetramethylolmethane.
7. according to the preparation method of a kind of new polyester polyvalent alcohol described in claim 1, it is characterized in that: the massfraction that the catalyzer in described step (1) accounts for blend is 0.3% ~ 1%.
8. a new polyester polyvalent alcohol, is characterized in that: obtained by the preparation method described in claim arbitrary in claim 1 ~ 7.
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| CN104650325B (en) | 2016-08-17 |
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