CN114062357A - Method for rapidly detecting polyether raw material sugar - Google Patents
Method for rapidly detecting polyether raw material sugar Download PDFInfo
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- CN114062357A CN114062357A CN202111536480.XA CN202111536480A CN114062357A CN 114062357 A CN114062357 A CN 114062357A CN 202111536480 A CN202111536480 A CN 202111536480A CN 114062357 A CN114062357 A CN 114062357A
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- raw material
- sugar
- material sugar
- polyether
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
Abstract
The invention belongs to the technical field of polyether polyol, and particularly relates to a method for rapidly detecting polyether raw material sugar. The method comprises the following steps: (1) adding polyalcohol, raw material sugar and hydroxide of alkali metal into a container for mixing; (2) heating the mixed material obtained in the step (1) under stirring at the temperature of 80-110 ℃; (3) and after heating for 30-50 minutes, observing the color change of the material, if the color change is not obvious or the color change reaches yellowish, considering that the raw material sugar is qualified and usable, and when the color value is reddish brown or black, considering that the raw material sugar is unqualified and cannot be used. The detection process is rapid and safe, and the operation method is simple and convenient; the raw material sugar detected to be qualified by the method is applied to the synthesis of polyether polyol, and the polyurethane foam prepared by the polyether polyol has high quality and good heat preservation effect.
Description
Technical Field
The invention belongs to the technical field of polyether polyol, and particularly relates to a method for rapidly detecting polyether raw material sugar.
Background
The polyurethane is widely applied to the field of buildings, particularly used for building heat preservation, can obviously improve the heat preservation performance of the buildings, reduces the energy waste and realizes low carbon and environmental protection. In recent years, the state has new requirements on low-carbon emission of building heat preservation, and the polyurethane is widely applied to the building heat preservation industry, the cold chain industry and the like in China and is also widely used in the household appliance industry.
The existing production of polyurethane monomer polyether generally adopts intermittent kettle type production, and the quality of polyether polyol of a product is low and the color value is high (larger than 15GD) due to the index influence of monomer polyether raw materials in the production process, so that the foam performance of a part of products is reduced in the process of preparing polyurethane foam, thereby not only causing pollution, but also wasting resources.
The existing production method has new requirements for raw material sugar detection: (1) the raw material sugar detection requirement is fast and accurate; (2) qualitative analysis gives whether it can be used. In addition, the unqualified raw material sugar can cause high hydroxyl value and color value of the product, and possible side reactions can occur to influence the performance of the polyurethane foam. At present, with the improvement of national building energy-saving requirements, the consumption of polyether polyol is gradually increased. With the gradual increase of the demand and the yield of the polyurethane monomer polyether, the problem of rapid detection of polyether raw material sugar needs to be solved urgently, the quality of polyurethane foam is influenced by side reactants, negative influence is brought to environmental protection, and the using amount of polyurethane is reduced.
For this reason, there is a continuing need in the art to develop a rapid detection method for the qualitative detection of sucrose reducing sugars.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for rapidly detecting polyether raw material sugar, which has the advantages of rapid and safe detection process and simple and convenient operation method; the raw material sugar detected to be qualified by the method is applied to the synthesis of polyether polyol, and the polyurethane foam prepared by the polyether polyol has high quality and good heat preservation effect.
The method for rapidly detecting the polyether raw material sugar comprises the following steps:
(1) adding polyalcohol, raw material sugar and hydroxide of alkali metal into a container for mixing;
(2) heating the mixed material obtained in the step (1) under stirring at the temperature of 80-110 ℃;
(3) and after heating for 30-50 minutes, observing the color change of the material, if the color change is not obvious or the color change reaches yellowish, considering that the raw material sugar is qualified and usable, and when the color value is reddish brown or black, considering that the raw material sugar is unqualified and cannot be used.
Wherein:
the container is a beaker, and can be a 150ml beaker.
The polyalcohol is one of diethylene glycol, glycerol, ethylene glycol or propylene glycol, and preferably diethylene glycol.
The raw material sugar is octa-hydroxyl sugar. Including one of sucrose or beet sugar.
The hydroxide of the alkali metal is potassium hydroxide, and solid potassium hydroxide is preferred.
The mass ratio of the polyhydric alcohol (diethylene glycol), the raw material sugar and the alkali metal hydroxide (potassium hydroxide) is 50:40:1-2.5, preferably 50:40: 1.5.
Preferably, after heating for 30 minutes, observing the color change of the material, if no obvious change or slight yellow is achieved, the raw material sugar is considered to be qualified and usable, and if the color value is reddish brown or black, the raw material sugar is considered to be unqualified and cannot be used.
Compared with the prior art, the invention has the following beneficial effects:
the method for rapidly detecting the polyether raw material sugar overcomes the problem of tedious detection of the monomer polyether raw material, can obviously and rapidly detect the raw material sugar of the polyether polyol, can avoid the waste of the raw material in the production process of the polyether polyol, is safe in detection process and simple and convenient in operation method, and the polyurethane polyether polyol prepared by the method has high quality and good heat preservation effect.
Detailed Description
The method for rapidly detecting the polyether raw material sugar comprises the following steps:
stirring raw materials of sugar, diethylene glycol and KOH solid according to a proportion in a glass beaker (150ml) with a heating device, continuously heating to 80-110 ℃, observing the change of color values under the stirring state, and keeping the time for 30-50 minutes; observing the color value, and judging the raw material sugar to be qualified if the color value is a mixture with no color change or slight yellow, and judging the raw material sugar to be unqualified if the color value is darker brown, deep reddish brown and black brown, and the raw material sugar cannot be used for producing polyether polyol.
At present, no related raw material detection is applied to polyether polyol synthesis, and the detection method can achieve the purpose of rapid detection.
In one embodiment, the polyol may be diethylene glycol, glycerol, ethylene glycol, propylene glycol, and the like, as commonly used in the art, preferably diethylene glycol.
The KOH may be an alkali metal hydroxide commonly used in the art.
In one embodiment, the detection temperature is preferably 80-110 ℃.
In one embodiment, the reaction pressure is atmospheric pressure.
And (3) reacting the qualified raw material sugar with epoxide to prepare the polycarboxylate water reducing agent monomer polyether.
In the preparation method of the polycarboxylic acid water reducing agent monomeric polyether, the epoxide can be various epoxides conventionally used in the field, preferably one or more of ethylene oxide and propylene oxide (mainly ethylene oxide and propylene oxide are used). In the preparation method of the polycarboxylic acid water reducer monomeric polyether, the method can be carried out according to the conventional method in the field, and the conventional conditions and steps of the reaction in the field can be referred to for each reaction condition and step. The following conditions are preferred in the present invention: the reaction temperature is preferably 140 ℃ or lower.
In the present invention, the term "color value" refers to the Gardner number, represented by GD.
The above preferred conditions can be arbitrarily combined to obtain preferred embodiments of the present invention without departing from the common general knowledge in the art.
The reagents and starting materials used in the present invention are commercially available.
The technical solutions of the present application will be clearly and completely described below with reference to the embodiments of the present application. The reagents and raw materials used are commercially available unless otherwise specified. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
Example 1
The raw material detection formula comprises: 50 parts of raw material sugar (cane sugar), 40 parts of diethylene glycol and 1.5 parts of solid potassium hydroxide.
The detection method comprises the following steps: adding 50 parts of raw material sugar into a 150ml beaker with a heating device, adding 40 parts of diethylene glycol and 1.5 parts of solid potassium hydroxide, stirring and heating, when the temperature reaches 90 ℃, the color value is unchanged within 30 minutes, the raw material is considered to be qualified, and meanwhile, the content of reducing sugar of the sugar is detected, and the corresponding numerical value is less than 0.1g/100 g.
Example 2
The raw material detection formula comprises: 50 parts of raw material sugar (beet sugar), 40 parts of glycerol (glycerin) and 1.5 parts of solid potassium hydroxide.
The detection method comprises the following steps: adding 50 parts of raw material sugar into a 150ml beaker with a heating device, adding 40 parts of glycerol and 1.5 parts of solid potassium hydroxide, stirring and heating, when the temperature reaches 110 ℃, the internal color value becomes yellowish in 30 minutes, the raw material is considered to be qualified, and meanwhile, the content of reducing sugar of the sugar is detected, and the corresponding numerical value is less than 0.1g/100 g.
Example 3
The raw material detection formula comprises: 50 parts of raw material sugar (cane sugar), 40 parts of ethylene glycol and 1.5 parts of solid potassium hydroxide.
The detection method comprises the following steps: 50 parts of raw material sugar is added into a 150ml beaker with a heating device, 40 parts of diethylene glycol and 1.5 parts of solid potassium hydroxide are added, the mixture is stirred and heated, when the temperature reaches 80 ℃, the color value changes into brownish red within 30 minutes, the raw material is considered unqualified, and the content of reducing sugar of the sugar is detected, wherein the corresponding numerical value is 0.12g/100 g.
Example 4
The raw material detection formula comprises: 50 parts of raw material sugar (cane sugar), 40 parts of diethylene glycol and 2.5 parts of solid potassium hydroxide.
The detection method comprises the following steps: adding 50 parts of raw material sugar into a 150ml beaker with a heating device, adding 40 parts of diethylene glycol and 2.5 parts of solid potassium hydroxide, stirring and heating, when the temperature reaches 100 ℃, the color value becomes yellowish within 50 minutes, the raw material is considered to be qualified, and meanwhile, the content of reducing sugar of the sugar is detected, and the corresponding numerical value is less than 0.1g/100 g.
Example 5
Adding raw material sugar detected in example 1 into a clean reaction kettle, introducing 120 parts of propylene oxide at 110 ℃ according to a polyether polyol synthesis method, keeping the reaction temperature for curing for one hour, and detecting the color value of polyether polyol, 6GD and the hydroxyl value of 415mg KOH/g after the curing. According to 100 parts of polyether polyol, 2 parts of silicone oil, 1.5 parts of water, 25 parts of foaming agent and isocyanate (PAPI) are mixed and foamed according to a ratio of 1:1.1 to prepare polyurethane foam, and the thermal conductivity coefficient of the product is 0.20.
Example 6
Adding raw material sugar detected in the example 3 into a clean reaction kettle, introducing 130 parts of propylene oxide at 110 ℃ according to a polyether polyol synthesis method, keeping the reaction temperature for curing for one hour, and detecting the color value of polyether polyol, 15GD and the hydroxyl value of 430mg KOH/g after the curing. Mixing 100 parts of polyether polyol, 2 parts of silicone oil, 1.5 parts of water, 25 parts of foaming agent and isocyanate (PAPI) according to a ratio of 1:1.1 for foaming to prepare polyurethane foam, wherein the thermal conductivity coefficient of the product is 0.25; the polyether product has dark black appearance and high foam heat conductivity coefficient.
Claims (8)
1. A method for rapidly detecting polyether raw material sugar is characterized by comprising the following steps: the method comprises the following steps:
(1) adding polyalcohol, raw material sugar and hydroxide of alkali metal into a container for mixing;
(2) heating the mixed material obtained in the step (1) under stirring at the temperature of 80-110 ℃;
(3) and after heating for 30-50 minutes, observing the color change of the material, if the color change is not obvious or the color change reaches yellowish, considering that the raw material sugar is qualified and usable, and when the color value is reddish brown or black, considering that the raw material sugar is unqualified and cannot be used.
2. The method for rapidly detecting the polyether raw material sugar as claimed in claim 1, wherein: the polyalcohol is one of diethylene glycol, glycerol, ethylene glycol or propylene glycol.
3. The method for rapidly detecting the polyether raw material sugar according to claim 1 or 2, wherein: the polyol is diethylene glycol.
4. The method for rapidly detecting the polyether raw material sugar as claimed in claim 1, wherein: the raw material sugar is octahydroxy sugar.
5. The method for rapidly detecting the polyether raw material sugar according to claim 1 or 4, wherein: the raw material sugar is one of sucrose or beet sugar.
6. The method for rapidly detecting the polyether raw material sugar as claimed in claim 1, wherein: the hydroxide of an alkali metal is potassium hydroxide.
7. The method for rapidly detecting the polyether raw material sugar as claimed in claim 5, wherein: the potassium hydroxide is solid potassium hydroxide.
8. The method for rapidly detecting the polyether raw material sugar as claimed in claim 1, wherein: the mass ratio of the polyhydric alcohol, the raw material sugar and the hydroxide of the alkali metal is 50:40: 1-2.5.
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| WO2001073407A2 (en) * | 2000-03-29 | 2001-10-04 | The Dow Chemical Company | Method for the determination of an acid or a base in a non-aqueous liquid |
| WO2013025616A1 (en) * | 2011-08-15 | 2013-02-21 | Receptors Llc | Competitive binding dendrimer-based system for analyte detection |
| CN104004178A (en) * | 2014-04-19 | 2014-08-27 | 上海东大化学有限公司 | Sucrose polyether polyol, preparation method and application thereof |
| CN105601902A (en) * | 2016-01-14 | 2016-05-25 | 浙江皇马科技股份有限公司 | Synthetic method of sucrose polyoxypropylene |
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| CN108020515A (en) * | 2017-11-28 | 2018-05-11 | 山东诺威新材料有限公司 | Test method of the saccharide raw material to polyether product colour and stability influence |
| EP3549670A1 (en) * | 2018-04-06 | 2019-10-09 | Covestro Deutschland AG | Manufacturing method for a polyurethane-poly(meth)acrylate resin |
| CN110982058A (en) * | 2019-12-25 | 2020-04-10 | 荆晓东 | Preparation method of sucrose ester polyether polyol |
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2021
- 2021-12-15 CN CN202111536480.XA patent/CN114062357A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB982280A (en) * | 1962-05-17 | 1965-02-03 | Allied Chem | New polyethers and polyurethane foams derived from them |
| CN1033522A (en) * | 1987-12-17 | 1989-06-28 | 沈阳市石油化工设计研究院 | A kind of synthetic method of polyether glycol |
| WO2001073407A2 (en) * | 2000-03-29 | 2001-10-04 | The Dow Chemical Company | Method for the determination of an acid or a base in a non-aqueous liquid |
| WO2013025616A1 (en) * | 2011-08-15 | 2013-02-21 | Receptors Llc | Competitive binding dendrimer-based system for analyte detection |
| CN104004178A (en) * | 2014-04-19 | 2014-08-27 | 上海东大化学有限公司 | Sucrose polyether polyol, preparation method and application thereof |
| CN105601902A (en) * | 2016-01-14 | 2016-05-25 | 浙江皇马科技股份有限公司 | Synthetic method of sucrose polyoxypropylene |
| CN105954278A (en) * | 2016-06-16 | 2016-09-21 | 江西出入境检验检疫局检验检疫综合技术中心 | Rapid determination method for content of total sugar in dry red wine |
| CN108020515A (en) * | 2017-11-28 | 2018-05-11 | 山东诺威新材料有限公司 | Test method of the saccharide raw material to polyether product colour and stability influence |
| EP3549670A1 (en) * | 2018-04-06 | 2019-10-09 | Covestro Deutschland AG | Manufacturing method for a polyurethane-poly(meth)acrylate resin |
| CN110982058A (en) * | 2019-12-25 | 2020-04-10 | 荆晓东 | Preparation method of sucrose ester polyether polyol |
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