CN104860794B - The method that the cracking of a kind of pentitol produces low molecular weight polyols - Google Patents
The method that the cracking of a kind of pentitol produces low molecular weight polyols Download PDFInfo
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- CN104860794B CN104860794B CN201510270942.6A CN201510270942A CN104860794B CN 104860794 B CN104860794 B CN 104860794B CN 201510270942 A CN201510270942 A CN 201510270942A CN 104860794 B CN104860794 B CN 104860794B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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Abstract
The invention discloses the method that the cracking of a kind of pentitol produces low molecular weight polyols.The method comprises the following steps: xylitol solution is heated to 35 40 DEG C by (1) at reduced pressure conditions, removes moisture, is slowly added dropwise the salt acid for adjusting pH value of the 1mol/L xylitol solution to 5.5, after being concentrated under agitation；(2) add platinum-rhodium alloy catalyst and zinc powder, 130 145 DEG C, be passed through neon under the conditions of pressure 10 12Mpa, react 8 14 hours, the mixture obtained is separated, distill and obtain ethylene glycol, propylene glycol, glycerol, butanediol and pentanediol.
Description
Technical field
The invention belongs to polyhydric alcohol preparation field, the method producing low molecular weight polyols particularly to the cracking of a kind of pentitol.
Background technology
Pentose (pentose), contains the sugar of 5 carbon atoms in a molecule.Most important in pentose have ribose (aldose), deoxyribose (aldose) and ribulose (ketose), and ribose and deoxyribose are the important component of nucleic acid；Ribulose is important intermediate metabolites, also known as xylose.
Pentitol, has another name called xylitol or pentite, is a kind of five-state controller, go for the sweeting agent of the food such as chewing gum, chocolate, hard sugar, pentitol metabolism in vivo need not insulin participation simultaneously, and blood glucose value will not be made to raise, can be as the sweeting agent of food with low sugar content.Additionally, xylitol is a kind of polyhydric alcohol, there is moisture absorption function, can use as the moistening regulator of toiletries, human body skin is had no stimulation.
The preparation of existing low molecular weight polyols is mainly obtained by the Pintsch process of the Fossil fuels such as oil, owing to the non-renewable of fossil feedstock and the conversion ratio being cracked into low-molecular-weight alcohols are relatively low, the method preparing raw material using Fossil fuel as low-molecular-weight alcohol is made to be limited by very large.
Summary of the invention
For above-mentioned demand, invention especially provides the method that the cracking of a kind of pentitol produces low molecular weight polyols.Low molecular weight polyols is prepared by the method, its low cost, and preparation technology is simple.
The purpose of the present invention can be achieved through the following technical solutions:
The method that the cracking of a kind of pentitol produces low molecular weight polyols, the method comprises the following steps:
(1) xylitol solution is heated to 35-40 DEG C at reduced pressure conditions, removes moisture, be slowly added dropwise the salt acid for adjusting pH value of the 1mol/L xylitol solution to 5.5, after being concentrated under agitation；
(2) add platinum-rhodium alloy catalyst and zinc powder, 180-195 DEG C, be passed through neon under the conditions of pressure 10-12Mpa, react 8-14 hour, the mixture obtained is separated, distill and obtain ethylene glycol, propylene glycol, glycerol, butanediol and pentanediol.
The consumption of described platinum-rhodium alloy catalyst is the 0.01-0.2wt% of the xylitol solution after concentrating.
The process of described separation includes centrifugal and filters.
In described xylitol solution, the mass concentration of xylitol is 12-55%.
In xylitol solution after described concentration, the mass concentration of xylitol is more than 85%.
The consumption of described zinc powder is the 0.01-0.02wt% of the xylitol solution after concentrating.
Also include before described xylitol solution heating under reduced pressure that adding activated carbon decolours to xylitol solution.
The pressure of described reduced pressure is 0.2-0.9Mpa.
The present invention compared with prior art, its
Beneficial effect
For
:
(1) present invention produces low molecular weight polyols by pentitol cracking, and its raw material preparing low-molecular-weight alcohol is simple and easy to get, low cost.
(2) method that the pentitol cracking of the present invention produces low molecular weight polyols, its conversion ratio is higher than the cracking of Fossil fuel.
(3) preparation method of the present invention is simple, it is easy to industrialized production.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1
(1) the xylitol solution 1000kg of 55wt% will add activated carbon, after stirring 15 minutes at 60 DEG C, filter；
(2) being heated to 35 DEG C under the conditions of 0.5Mpa, remove moisture, be slowly added dropwise the salt acid for adjusting pH value of 1mol/L under agitation to 5.5, the xylitol solution after being concentrated, wherein the mass concentration of the xylitol solution after concentration is 85%；
(3) add platinum-rhodium alloy 0.1kg and zinc powder 0.2kg, 180 DEG C, be passed through neon under the conditions of pressure 12Mpa, react 8 hours, the mixture that will obtain filters, and distills and obtains ethylene glycol, propylene glycol, glycerol, butanediol and pentanediol.
Embodiment 2
(1) the xylitol solution 1000kg of 12wt% will add activated carbon, after stirring 8 minutes at 80 DEG C, filter；
(2) being heated to 35 DEG C under the conditions of 0.2Mpa, remove moisture, be slowly added dropwise the salt acid for adjusting pH value of 1mol/L under agitation to 5.5, the xylitol solution after being concentrated, wherein the mass concentration of the xylitol solution after concentration is 95%；
(3) add platinum-rhodium alloy 0.1kg and zinc powder 0.1kg, 195 DEG C, be passed through neon under the conditions of pressure 10Mpa, react 10 hours, the mixture obtained is centrifuged, the liquid obtained is distilled and obtains ethylene glycol, propylene glycol, glycerol, butanediol and pentanediol.
Embodiment 3
(1) the xylitol solution 1000kg of 20wt% will add activated carbon, after stirring 8 minutes at 60 DEG C, filter；
(2) being heated to 40 DEG C under the conditions of 0.9Mpa, remove moisture, be slowly added dropwise the salt acid for adjusting pH value of 1mol/L under agitation to 5.5, the xylitol solution after being concentrated, wherein the mass concentration of the xylitol solution after concentration is 89%；
(3) add platinum-rhodium alloy 2kg and zinc powder 0.2kg, 185 DEG C, be passed through neon under the conditions of pressure 12Mpa, react 14 hours, the mixture that will obtain filters, and distills and obtains ethylene glycol, propylene glycol, glycerol, butanediol and pentanediol.
Embodiment 1-3 obtains the productivity of each low molecular weight polyols by gas chromatographic detection calculating, the most as shown in table 1.
Table 1
| Polyhydric alcohol | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Ethylene glycol productivity | 32.1% | 29.5% | 30.1% |
| Propylene glycol productivity | 44.1% | 45.6% | 42.9% |
| Glycerol productivity | 11.9% | 12.1% | 14.4% |
| Butanediol productivity | 6.9% | 9.5% | 7.2% |
| Pentanediol productivity | 5.0% | 3.3% | 5.4% |
The invention is not restricted to embodiment here, those skilled in the art should be within protection scope of the present invention according to the announcement of the present invention, the improvement made without departing from scope and amendment.
Claims (8)
1. the method that a pentitol cracking produces low molecular weight polyols, it is characterised in that the method comprises the following steps:
(1) xylitol solution is heated to 35-40 DEG C at reduced pressure conditions, removes moisture, be slowly added dropwise the salt acid for adjusting pH value of the 1mol/L xylitol solution to 5.5, after being concentrated under agitation；
(2) add platinum-rhodium alloy catalyst and zinc powder, 180-195 DEG C, be passed through neon under the conditions of pressure 10-12Mpa, react 8-14 hour, the mixture obtained is separated, distill and obtain ethylene glycol, propylene glycol, glycerol, butanediol and pentanediol.
The method that the most according to claim 1, pentitol cracking produces low molecular weight polyols, it is characterised in that the consumption of described platinum-rhodium alloy catalyst is the 0.01-0.2wt% of the xylitol solution after concentrating.
The method that the most according to claim 1, pentitol cracking produces low molecular weight polyols, it is characterised in that the process of described separation includes centrifugal and filters.
The method that the most according to claim 1, pentitol cracking produces low molecular weight polyols, it is characterised in that in described xylitol solution, the mass concentration of xylitol is 12-55%.
The method that the most according to claim 1, pentitol cracking produces low molecular weight polyols, it is characterised in that in the xylitol solution after described concentration, the mass concentration of xylitol is more than 85%.
The method that the most according to claim 1, pentitol cracking produces low molecular weight polyols, it is characterised in that the consumption of described zinc powder is the 0.01-0.02wt% of the xylitol solution after concentrating.
The method that the most according to claim 1, pentitol cracking produces low molecular weight polyols, it is characterised in that also include before described xylitol solution heating under reduced pressure that adding activated carbon decolours to xylitol solution.
The method that the most according to claim 1, pentitol cracking produces low molecular weight polyols, it is characterised in that the pressure of described reduced pressure is 0.2-0.9Mpa.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103360205A (en) * | 2006-05-08 | 2013-10-23 | 维仁特公司 | Methods and systems for generating polyols |
| CN103833513A (en) * | 2012-11-26 | 2014-06-04 | 中国科学院大连化学物理研究所 | Method for preparing 1, 2-propanediol by adopting jerusalem artichoke as raw material in direct catalytic conversion |
| CN104557461A (en) * | 2014-12-31 | 2015-04-29 | 上海交通大学 | Method for preparing 1,2-propylene glycol through adopting metal for hydrothermal reduction of carbohydrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101205897B1 (en) * | 2010-04-19 | 2012-11-29 | 한국과학기술연구원 | The noble metal based catalyst supported on complex metal oxide and the method for the producing of 1,2-propanediol |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103360205A (en) * | 2006-05-08 | 2013-10-23 | 维仁特公司 | Methods and systems for generating polyols |
| CN103833513A (en) * | 2012-11-26 | 2014-06-04 | 中国科学院大连化学物理研究所 | Method for preparing 1, 2-propanediol by adopting jerusalem artichoke as raw material in direct catalytic conversion |
| CN104557461A (en) * | 2014-12-31 | 2015-04-29 | 上海交通大学 | Method for preparing 1,2-propylene glycol through adopting metal for hydrothermal reduction of carbohydrate |
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