CN108020515A - Test method of the saccharide raw material to polyether product colour and stability influence - Google Patents
Test method of the saccharide raw material to polyether product colour and stability influence Download PDFInfo
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- CN108020515A CN108020515A CN201711217408.4A CN201711217408A CN108020515A CN 108020515 A CN108020515 A CN 108020515A CN 201711217408 A CN201711217408 A CN 201711217408A CN 108020515 A CN108020515 A CN 108020515A
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- raw material
- saccharide raw
- test method
- product colour
- stability influence
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/29—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using visual detection
- G01N21/293—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using visual detection with colour charts, graduated scales or turrets
Abstract
A kind of test method the present invention relates to saccharide raw material to polyether product colour and stability influence, belongs to polyether polyol detection and analysis field.This method comprises the following steps：Aqueous slkali is prepared with ultra-pure water；Saccharide raw material is added in aqueous slkali, is warming up to 90 150 DEG C of beginning timing；Syrup is obtained after timing, syrup is poured into colorimetric cylinder, is tested.The rule of this method detection is consistent with the index rule of the polyether polyol of carbohydrate synthesis, and method is simple, the cycle is short, easily operated, and experimental result is reproducible.
Description
Technical field
A kind of test method the present invention relates to saccharide raw material to polyether product colour and stability influence, it is more to belong to polyethers
First alcohol tests and analyzes field.
Background technology
Carbohydrate due to its is cheap and easy to get, in molecular structure containing multiple hydroxyl and polymerization activities it is moderate the features such as,
One of primary raw material as polyether polyol initiator, including the polyol such as sucrose, sorbierite, xylitol.But by
There is larger shadow in the different colours and stability to Contents In Polyether Polyol of batch wise differences, production technology and quality
Ring, therefore the detection verification of raw material is often vital one in polyether polyol synthesis.Currently for carbohydrate initiator
On polyether polyol influence common detection methods be：Pass through polymerisation synthesizing polyether glycol, contrast polyether polyol production
Product index stability judges the stability of carbohydrate initiator.This method cycle is long, technological requirement is high, disturbing factor is more, time-consuming
Effort.Therefore, it is badly in need of a kind of method of simple possible, improves above-mentioned raw materials verification efficiency, and the effort for it of each producer
Direction.
The content of the invention
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of saccharide raw material to polyether product colour and stabilization
Property influence test method, it is simple and easy to do, shorten proving period, improve work efficiency.
To rigid-foam polyether with aqueous slkali is added in raw polyol, heat under certain condition and pass through solution after heating
Colour judges the stability of raw produce.
A kind of saccharide raw material of the present invention is including as follows to the test method of polyether product colour and stability influence
Step：
(1) aqueous slkali is prepared with ultra-pure water；
(2) saccharide raw material is added in aqueous slkali, is warming up to 90-150 DEG C of beginning timing；
(3) syrup is obtained after timing, syrup is poured into colorimetric cylinder, is tested.
Wherein；
The mass ratio of ultra-pure water and glycogen material is 1~3:3~12.
The concentration of aqueous slkali is 2%-20%.
Alkali is in sodium hydroxide, potassium hydroxide, calcium hydroxide, natrium carbonicum calcinatum, sodium acid carbonate, potassium carbonate or saleratus
One or more.
Step (2) timing time is 0.2-1.5h.
Nitrogen displacement is carried out before step (2) heating.
The index of the ultra-pure water refers to China national lab analysis water supply standard (GB6682-92).
Method in the syrup colourity test reference GB/T22295-2008 standards.
Compared with prior art, the present invention has the following advantages：
(1) after the present invention to glucide by carrying out alkali soluble experiment, the colourity of solution changes to examine after observation experiment
Influence of the saccharide raw material to polyether polyol colour and product stability, different impurities content, the carbohydrate warp of different process production
After crossing this method detection, colour otherness is obvious；
(2) rule of this method detection is consistent with the index rule of the polyether polyol of carbohydrate synthesis；
(3) detection method is simple, the cycle is short, easily operated, and experimental result is reproducible.
Embodiment
With reference to embodiment, the present invention will be further described.
Embodiment 1
It is being equipped with the three-necked flask of magnetic stirring apparatus, thermometer, condensing unit and nitrogen protection device, is adding hydrogen-oxygen
Change sodium 3g, ultra-pure water 30g, nitrogen displacement 3 times.Make sodium hydroxide dissolving completely and keep stable, to eliminate sodium hydroxide in itself
Quality problems to next step detect caused by Color influences.90g sucrose is added into three-necked flask, is opened after nitrogen displacement 3 times
Begin to stir, rotating speed 20r/s, starts to warm up at this time, starts timing when temperature rises to 130 DEG C, stops heating after 40min, take out
Three-necked flask, places cooling.Syrup is transferred in colorimetric cylinder after solution cooling.Range estimation ratio is carried out with Gardner's glass colour code
Compared with the color with certain immediate Color standard number representing sample of sample color.Test index is as follows：
Reaction and detection time：70min
Colour (Jia Shi colorimeters measure)：7
It is as follows with the Sucrose synthesis polyether polyol used in the present embodiment 1, its product index：
Hydroxyl value：452mgKOH/g
Viscosity (25 DEG C)：8560mPas
Colour：3
Synthesising reacting time：16h.
Embodiment 2
It is being equipped with the three-necked flask of magnetic stirring apparatus, thermometer, condensing unit and nitrogen protection device, is adding hydrogen-oxygen
Change potassium 5g, ultra-pure water 40g, nitrogen displacement 3 times.Make potassium hydroxide dissolving completely and keep stable, to eliminate potassium hydroxide in itself
Quality problems to next step detect caused by Color influences.80g sucrose is added into three-necked flask, is opened after nitrogen displacement 3 times
Begin to stir, rotating speed 25r/s, starts to warm up at this time, starts timing when temperature rises to 130 DEG C, stops heating after 40min, take out
Three-necked flask, places cooling.Syrup is transferred in colorimetric cylinder after solution cooling.Range estimation ratio is carried out with Gardner's glass colour code
Compared with the color with certain immediate Color standard number representing sample of sample color.Test index is as follows：
Reaction and detection time：70min
Colour (Jia Shi colorimeters measure)：9
It is as follows with the Sucrose synthesis polyether polyol used in the present embodiment 2, its product index：
Hydroxyl value：448mgKOH/g
Viscosity (25 DEG C)：8000mPas
Colour：4
Synthesising reacting time：16h.
Embodiment 3
It is being equipped with the three-necked flask of magnetic stirring apparatus, thermometer, condensing unit and nitrogen protection device, is adding hydrogen-oxygen
Change potassium 2g, ultra-pure water 20g, nitrogen displacement 3 times.Make potassium hydroxide dissolving completely and keep stable, to eliminate potassium hydroxide in itself
Quality problems to next step detect caused by Color influences.The addition 60g sorbierites into three-necked flask, nitrogen displacement 3 times, this
When start to warm up, start timing when temperature rises to 130 DEG C, stop heating after 40min, take out three-necked flask, place cooling.Treat
Syrup is transferred in colorimetric cylinder after solution cooling.Range estimation comparison is carried out with Gardner's glass colour code, most to be connect with sample color
The color of certain near Color standard number representing sample.Test index is as follows：
Reaction and detection time：70min
Colour (Jia Shi colorimeters measure)：5
It is as follows with the sorbierite synthesizing polyether glycol used in the present embodiment 3, its product index：
Hydroxyl value：460mgKOH/g
Viscosity (25 DEG C)：13000mPas
Colour：2
Synthesising reacting time：16h.
Colour index comparison is carried out to polysaccharide raw material and polyether polyol prepared therefrom, the results are shown in Table 1.
The colour of 1 saccharide raw material of table and polyether product
| Colour | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Saccharide raw material | 7 | 9 | 5 |
| Polyether polyol | 3 | 4 | 2 |
As can be seen from the table, consistent regularity is presented in the colour index of the colour of saccharide raw material and polyether polyol.
Claims (6)
1. a kind of saccharide raw material is to the test method of polyether product colour and stability influence, it is characterised in that：Including following step
Suddenly：
(1) aqueous slkali is prepared with ultra-pure water；
(2) saccharide raw material is added in aqueous slkali, is warming up to 90-150 DEG C of beginning timing；
(3) syrup is obtained after timing, syrup is poured into colorimetric cylinder, is tested.
2. saccharide raw material according to claim 1 is to the test method of polyether product colour and stability influence, its feature
It is：The mass ratio of ultra-pure water and glycogen material is 1~3:3~12.
3. saccharide raw material according to claim 1 is to the test method of polyether product colour and stability influence, its feature
It is：The concentration of aqueous slkali is 2%-20%.
4. saccharide raw material according to claim 1 is to the test method of polyether product colour and stability influence, its feature
It is：Alkali is in sodium hydroxide, potassium hydroxide, calcium hydroxide, natrium carbonicum calcinatum, sodium acid carbonate, potassium carbonate or saleratus
It is one or more.
5. saccharide raw material according to claim 1 is to the test method of polyether product colour and stability influence, its feature
It is：Step (2) timing time is 0.2-1.5h.
6. saccharide raw material according to claim 1 is to the test method of polyether product colour and stability influence, its feature
It is：Nitrogen displacement is carried out before step (2) heating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201711217408.4A CN108020515A (en) | 2017-11-28 | 2017-11-28 | Test method of the saccharide raw material to polyether product colour and stability influence |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114062357A (en) * | 2021-12-15 | 2022-02-18 | 上海东大化学有限公司 | Method for rapidly detecting polyether raw material sugar |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106146823A (en) * | 2016-07-30 | 2016-11-23 | 淄博德信联邦化学工业有限公司 | The preparation method of pure crystalline sorbitol polyether polyol |
-
2017
- 2017-11-28 CN CN201711217408.4A patent/CN108020515A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106146823A (en) * | 2016-07-30 | 2016-11-23 | 淄博德信联邦化学工业有限公司 | The preparation method of pure crystalline sorbitol polyether polyol |
Non-Patent Citations (2)
| Title |
|---|
| 中华人员共和国国家质量监督检验检疫总局和中国国家标准化管理委员会: "《中华人民共和国国家标准》", 4 August 2008 * |
| 胡庆国等: "《浅谈对聚醚色值的影响因素》", 《山东化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114062357A (en) * | 2021-12-15 | 2022-02-18 | 上海东大化学有限公司 | Method for rapidly detecting polyether raw material sugar |
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Application publication date: 20180511 |
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