CN114989230A - Method for preparing maltitol - Google Patents
Method for preparing maltitol Download PDFInfo
- Publication number
- CN114989230A CN114989230A CN202210701944.6A CN202210701944A CN114989230A CN 114989230 A CN114989230 A CN 114989230A CN 202210701944 A CN202210701944 A CN 202210701944A CN 114989230 A CN114989230 A CN 114989230A
- Authority
- CN
- China
- Prior art keywords
- hydrogenation
- reaction
- maltitol
- kettle
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/02—Acyclic radicals, not substituted by cyclic structures
- C07H15/04—Acyclic radicals, not substituted by cyclic structures attached to an oxygen atom of the saccharide radical
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Saccharide Compounds (AREA)
Abstract
The invention belongs to the technical field of maltitol preparation, and relates to a method for preparing maltitol, which comprises the following steps: adding maltose syrup and a nickel catalyst into a hydrogenation kettle in proportion, starting a stirring device of the hydrogenation kettle to uniformly mix reaction substrates in the hydrogenation kettle, adjusting the initial pH value of the reaction to be 5.0-6.0 by using alkali liquor with the concentration of 5%, introducing hydrogen, controlling the temperature of the hydrogenation kettle to be 125-135 ℃ and the pressure to be 8.5-9.0 MPa, and carrying out hydrogenation reaction on the reaction substrates in the hydrogenation kettle for about 2.0-2.5 h; respectively injecting 5% NaOH solution at different reaction stages, and controlling the pH value of a reaction substrate to be 5.5-6.0 during hydrogenation reaction; after the hydrogenation reaction is finished, the reaction solution in the hydrogenation kettle is sequentially subjected to cooling, sedimentation and filtration treatment to obtain the maltitol solution. According to the invention, a carboxylic acid byproduct generated in the maltose hydrogenation reaction process is remarkably reduced by a sectional alkali injection mode, the maltose conversion rate and the content of maltitol in the hydrogenation solution are improved, and the production efficiency of maltitol is improved.
Description
Technical Field
The invention belongs to the technical field of maltitol preparation, and particularly relates to a method for preparing maltitol.
Background
Maltitol is widely used in the fields of chemical industry, food, medicine, etc. due to its excellent properties such as good acid-heat stability, low calorie, high sweetness, etc. The preparation of maltitol usually takes starch as raw material, alpha-amylase, beta-amylase and the like are adopted to carry out enzymolysis on the starch to form maltose syrup, and the maltose syrup is converted into the maltitol by skeletal nickel catalytic hydrogenation. However, during the hydrogenation reaction of maltose, carboxylic acid by-products such as gluconic acid are easily generated, so that nickel and aluminum in the skeletal nickel catalyst are dissolved into the maltose solution, thereby reducing the activity and stability of the catalyst, and the hydrolysis side reaction is further increased as the pH value of the solution is gradually decreased. For example, patent publication No. CN109336939A provides a method for adjusting the pH value during the reaction process by adding magnesium powder, but the magnesium powder in the process is added in advance at one time, it is difficult to control the hydrogenation reaction in a targeted manner, and the magnesium powder is flammable and explosive, which has potential safety hazard. Also, for example, patent publication No. CN110845303A discloses a method of single continuous alkali injection to increase the stability of the catalyst, reduce its consumption, increase the hydrogenation efficiency, and increase the substrate conversion rate. However, this method still has disadvantages: (1) the long time of single alkali injection can cause local over-alkali; (2) the carboxylic acid by-product is not effectively controlled.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing maltitol, which can remarkably reduce carboxylic acid by-products generated in the hydrogenation reaction process of maltose, improve the conversion rate of maltose and the content of maltitol in hydrogenated liquid and improve the production efficiency of maltitol by a sectional alkali injection mode.
The present invention is achieved by providing a method for producing maltitol, comprising the steps of:
step one, feeding: adding maltose syrup and a nickel catalyst into a hydrogenation kettle in proportion, and starting a stirring device of the hydrogenation kettle to uniformly mix reaction substrates in the hydrogenation kettle;
step two, adjusting the pH value: adjusting the initial pH value of the reaction to 5.0-6.0 by using alkali liquor with the concentration of 5%;
step three, hydrogenation: introducing hydrogen into the system obtained in the second step, controlling the temperature of the hydrogenation kettle to be 125-135 ℃ and the pressure to be 8.5-9.0 MPa, and carrying out hydrogenation reaction on a reaction substrate in the hydrogenation kettle for about 2.0-2.5 h;
step four, alkali is injected in sections: in the hydrogenation reaction process of the third step, NaOH solutions with the concentration of 5% are respectively injected into different reaction stages, and the pH value of a reaction substrate in the hydrogenation reaction is controlled to be 5.5-6.0;
step five, solid-liquid separation: and after the hydrogenation reaction is finished, sequentially cooling, settling and filtering the reaction solution in the hydrogenation kettle to obtain the maltitol solution.
Further, in the fourth step, the alkali injection times are divided into two or three times, and when the alkali injection times are two, the alkali injection time is set to be 5 min-10 min and 60 min-90 min of the hydrogenation reaction; and when the alkali injection times are three times, the alkali injection time is arranged in the 5 th-10 th min, the 60 th-70 th min and the 75 th-90 th min of the hydrogenation reaction, wherein the alkali injection time for the second time and the alkali injection time for the third time are at least separated by more than 10 min.
Further, the NaOH solution is stored in an alkali liquor tank in advance, the alkali liquor tank is communicated with a feed inlet of the hydrogenation kettle through an alkali conveying pipeline, and a flow meter for detecting the alkali conveying amount is arranged on the alkali conveying pipeline.
Compared with the prior art, the method for preparing maltitol has the following characteristics:
1. the method adopts a segmented alkali injection process for the first time, optimizes the process of preparing maltitol by hydrogenating maltose, and effectively reduces the generation of hydrogenation byproducts, so that the conversion rate of maltose is more than or equal to 99.4 percent and the content of maltitol is more than or equal to 87.3 percent.
2. In the adopted segmented alkali injection process, the alkali injection frequency is more than or equal to 2 times, and the time point of the second alkali injection is not earlier than 60min from the beginning of the hydrogenation reaction, under the condition, the amount of carboxylic acid by-products in the obtained maltitol is less than or equal to 0.30 percent, which is reduced by more than 82.7 percent compared with the prior art; meanwhile, the problem of loss of nickel and aluminum in the hydrogenation reaction process of the skeletal nickel catalyst is solved, the service life of the catalyst is prolonged, and the stability of the catalyst is improved.
3. The required sodium hydroxide is easy to obtain, the cost is low, and meanwhile, the sectional alkali injection process is simple, easy to operate and suitable for industrial production.
Drawings
FIG. 1 is a schematic diagram of the structure of a preferred embodiment of the system for preparing maltitol according to the invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects of the present invention more clearly understood, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to FIG. 1, a preferred embodiment of the method for preparing maltitol according to the present invention uses a system for preparing maltitol.
The system for preparing the maltitol comprises a hydrogenation kettle 1, an alkali liquor tank 2 and a flow meter 3. The hydrogenation kettle 1 is respectively provided with a feeding end and a discharging end, the feeding end is arranged at the upper part of the hydrogenation kettle 1, and the discharging end is arranged at the lower part of the hydrogenation kettle 1. The feed end is respectively provided with an alkali liquor feed port communicated with an alkali conveying pipeline 5, a hydrogen gas inlet communicated with a hydrogen pipeline 6, a maltose syrup feed port communicated with a syrup feed pipeline 7 and a nickel catalyst feed port communicated with a catalyst feed pipeline 8, and the discharge end is provided with a reaction solution discharge port communicated with a discharge pipeline 9. The flowmeter 3 is arranged on the alkali conveying pipeline 5, and the flowmeter 3 is used for detecting the alkali conveying flow. The other end of the alkali conveying pipeline 5 is communicated with a discharge hole of the alkali liquor tank 2. A stirring device 10 is provided in the hydrogenation reactor 1.
The method for preparing maltitol comprises the following steps:
step one, feeding: adding maltose syrup and nickel catalyst into the hydrogenation kettle 1 in proportion, and starting a stirring device 10 of the hydrogenation kettle 1 to uniformly mix reaction substrates in the hydrogenation kettle 1.
Step two, adjusting the pH value: adjusting the initial pH value of the reaction to 5.0-6.0 by using alkali liquor with the concentration of 5%.
Step three, hydrogenation: and (3) introducing hydrogen into the system obtained in the step two, controlling the temperature of the hydrogenation kettle 1 to be 125-135 ℃ and the pressure to be 8.5-9.0 MPa, and carrying out hydrogenation reaction on the reaction substrate in the hydrogenation kettle 1 for about 2.0-2.5 h.
Step four, alkali is injected in sections: and in the hydrogenation reaction process of the third step, NaOH solutions with the concentration of 5% are respectively injected into different reaction stages, and the pH value of a reaction substrate in the hydrogenation reaction is controlled to be 5.5-6.0.
Step five, solid-liquid separation: after the hydrogenation reaction is finished, the reaction solution in the hydrogenation kettle 1 is sequentially subjected to temperature reduction, sedimentation and filtration treatment to obtain the maltitol solution.
In the fourth step, the alkali is injected in sections twice or three times. When the alkali injection times are two, the alkali injection time is arranged in the 5 th-10 th min and the 60 th-90 th min of the hydrogenation reaction. And when the alkali injection times are three times, the alkali injection time is arranged in the 5 th-10 th min, the 60 th-70 th min and the 75 th-90 th min of the hydrogenation reaction, wherein the alkali injection time for the second time and the alkali injection time for the third time are at least separated by more than 10 min.
In the fourth step, the NaOH solution is stored in the lye tank 2 in advance, the lye tank 2 is communicated with the lye feed inlet of the hydrogenation kettle 1 through a lye conveying pipeline 5, and a flowmeter 3 for detecting the lye conveying amount is arranged on the lye conveying pipeline 5.
The process for the preparation of maltitol according to the invention is further illustrated by the following specific examples.
Example 1
An embodiment of the first process for the preparation of maltitol according to the invention comprises the following steps: adding 600mL of maltose syrup into a hydrogenation kettle 1, adding 14g/L of skeleton nickel catalyst, adjusting the pH value of a reaction substrate in the hydrogenation kettle 1 to 5.6, setting the hydrogenation reaction temperature to 130 ℃, the hydrogenation reaction pressure to 9MPa, reacting for 2.5h, carrying out solid-liquid separation on a reaction solution in the hydrogenation kettle 1 after the hydrogenation reaction is finished, and filtering to remove the nickel catalyst to obtain a maltitol solution; wherein, at the 10 th min and the 60 th min of the hydrogenation reaction, 5 percent sodium hydroxide solution is respectively injected into the reaction substrate at the flow rate of 3mL/min for 5 min; the pH of the reaction substrate was controlled to 5.7. In the obtained maltitol solution, the gluconic acid content was 0.25%, the maltitol content was 87.3%, and the maltose conversion rate was 99.4%.
Example 2
An embodiment of the second process for the preparation of maltitol according to the invention comprises the following steps: adding 600mL of maltose syrup into a hydrogenation kettle 1, adding 14g/L of skeleton nickel catalyst, adjusting the pH value of a reaction substrate in the hydrogenation kettle 1 to 5.8, setting the hydrogenation reaction temperature to 130 ℃, the hydrogenation reaction pressure to 9MPa, reacting for 2.5 hours, carrying out solid-liquid separation on a reaction solution in the hydrogenation kettle 1 after the hydrogenation reaction is finished, and filtering to remove the nickel catalyst to obtain a maltitol solution; wherein, at the 10 th min and the 90 th min of the hydrogenation reaction, 5% sodium hydroxide solution is respectively injected into the reaction substrate at the flow rate of 3mL/min for 5min, and the pH value of the reaction substrate is controlled to be 5.9. In the obtained maltitol solution, the content of gluconic acid was 0.13%, the content of maltitol was 88.5%, and the conversion rate of maltose was 99.5%.
Example 3
An example of the third process for preparing maltitol according to the invention comprises the following steps: adding 600mL of maltose syrup into a hydrogenation kettle 1, adding 14g/L of skeleton nickel catalyst, adjusting the pH value of a reaction substrate in the hydrogenation kettle 1 to 5.8, setting the hydrogenation reaction temperature to 130 ℃, the hydrogenation reaction pressure to 9MPa, reacting for 2.5h, carrying out solid-liquid separation on a reaction solution in the hydrogenation kettle 1 after the hydrogenation reaction is finished, and filtering to remove the nickel catalyst to obtain a maltitol solution; wherein, in the hydrogenation reaction of 10min, 60min and 75min, respectively injecting 5% sodium hydroxide solution into the reaction substrate at the flow rate of 3mL/min for 3 min; the pH of the reaction substrate was controlled to 5.9. In the obtained maltitol solution, the content of gluconic acid was 0.10%, the content of maltitol was 89.0%, and the conversion rate of maltose was 99.7%.
Example 4
An embodiment of the fourth process for the preparation of maltitol according to the invention comprises the following steps: adding 600mL of maltose syrup into a hydrogenation kettle 1, adding 14g/L of skeleton nickel catalyst, adjusting the pH value of a reaction substrate in the hydrogenation kettle 1 to 5.5, setting the hydrogenation reaction temperature to 130 ℃, the hydrogenation reaction pressure to 8.5MPa, reacting for 2.5h, carrying out solid-liquid separation on a reaction solution in the hydrogenation kettle 1 after the hydrogenation reaction is finished, and filtering to remove the nickel catalyst to obtain a maltitol solution; wherein, 5% sodium hydroxide solution is respectively injected into the reaction substrate for 3min at the flow rate of 3mL/min at the 10 th min, the 60 th min and the 90 th min of the hydrogenation reaction; the pH of the reaction substrate was controlled to 5.6. In the obtained maltitol solution, the content of gluconic acid was 0.18%, the content of maltitol was 88.1%, and the conversion rate of maltose was 99.5%.
Example 5
An embodiment of the fifth process for preparing maltitol according to the invention comprises the following steps: adding 3L of maltose syrup into a hydrogenation kettle 1, adding 14g/L of skeleton nickel catalyst, adjusting the pH value of a reaction substrate in the hydrogenation kettle 1 to 5.6, setting the hydrogenation reaction temperature to 130 ℃, the hydrogenation reaction pressure to 9MPa, reacting for 2 hours, carrying out solid-liquid separation on a reaction solution in the hydrogenation kettle 1 after the hydrogenation reaction is finished, and filtering to remove the nickel catalyst to obtain a maltitol solution; wherein, 5% sodium hydroxide solution is respectively injected into the reaction substrate for 5min at the flow rate of 15mL/min at the 10 th min and the 90 th min of the hydrogenation reaction; the pH of the reaction substrate was controlled to 5.7. In the obtained maltitol solution, the content of gluconic acid was 0.26%, the content of maltitol was 87.8%, and the conversion rate of maltose was 99.7%.
Example 6
An embodiment of the sixth method for producing maltitol of the present invention comprises the steps of: adding 3L of maltose syrup into a hydrogenation kettle 1, adding 14g/L of skeletal nickel catalyst, adjusting the pH value of a reaction substrate in the hydrogenation kettle 1 to 5.7, setting the hydrogenation reaction temperature to 130 ℃, the hydrogenation reaction pressure to 8.5MPa, reacting for 2 hours, carrying out solid-liquid separation on a reaction solution in the hydrogenation kettle 1 after the hydrogenation reaction is finished, and filtering to remove the nickel catalyst to obtain a maltitol solution; wherein, 5% sodium hydroxide solution is respectively injected into the reaction solution at the flow rate of 15mL/min for 3min at the 10 th min, the 60 th min and the 90 th min of the hydrogenation reaction; the pH of the reaction substrate was controlled to 5.8. In the obtained maltitol solution, the content of gluconic acid was 0.17%, the content of maltitol was 88.4%, and the conversion rate of maltose was 99.5%.
Example 7
An embodiment of the seventh method for preparing maltitol of the invention comprises the following steps: adding 600mL of maltose syrup into a hydrogenation kettle 1, adding 14g/L of skeleton nickel catalyst, adjusting the pH value of a reaction substrate in the hydrogenation kettle 1 to 5.0, setting the hydrogenation reaction temperature to 125 ℃, the hydrogenation reaction pressure to 9MPa, reacting for 2.5 hours, carrying out solid-liquid separation on a reaction solution in the hydrogenation kettle 1 after the hydrogenation reaction is finished, and filtering to remove the nickel catalyst to obtain a maltitol solution; wherein, at the 10 th min and the 60 th min of the hydrogenation reaction, respectively injecting 5% sodium hydroxide solution into the reaction substrate at the flow rate of 3mL/min for 5 min; the pH of the reaction substrate was controlled to 5.5. In the obtained maltitol solution, the gluconic acid content was 0.25%, the maltitol content was 87.3%, and the maltose conversion rate was 99.4%.
Example 8
An embodiment of the eighth method for preparing maltitol according to the invention comprises the following steps: adding 600mL of maltose syrup into a hydrogenation kettle 1, adding 14g/L of skeleton nickel catalyst, adjusting the pH value of a reaction substrate in the hydrogenation kettle 1 to 6.0, setting the hydrogenation reaction temperature to 135 ℃, the hydrogenation reaction pressure to 8.5MPa, reacting for 2.0h, carrying out solid-liquid separation on a reaction solution in the hydrogenation kettle 1 after the hydrogenation reaction is finished, and filtering to remove the nickel catalyst to obtain a maltitol solution; wherein, at the 10 th min and the 60 th min of the hydrogenation reaction, 5% sodium hydroxide solution is respectively injected into the reaction substrate at the flow rate of 3mL/min for 5min, and the pH value of the reaction substrate is controlled to be 6.0. In the obtained maltitol solution, the content of gluconic acid was 0.20%, the content of maltitol was 88.3%, and the conversion rate of maltose was 99.6%.
Comparative example 1
Comparative example of the first process for preparing maltitol according to the invention, comprising the following steps: adding 600mL of maltose syrup into a hydrogenation kettle 1, adding 12g/L of skeleton nickel catalyst, adjusting the pH value of a reaction substrate in the hydrogenation kettle 1 to 5.5, setting the hydrogenation reaction temperature to be 130 ℃, the hydrogenation reaction pressure to be 8MPa, reacting for 2 hours, carrying out solid-liquid separation on a reaction solution in the hydrogenation kettle 1 after the hydrogenation reaction is finished, and filtering to remove the nickel catalyst to obtain a maltitol solution; wherein, at the 10 th min of the hydrogenation reaction, 5% sodium hydroxide solution was injected into the reaction substrate at a flow rate of 3mL/min for 10min, respectively. In the obtained maltitol solution, the gluconic acid content was 2.60%, the maltitol content was 79.4%, and the maltose conversion rate was 95.8%.
In comparative example 1, a single alkali injection was used in the alkali injection process, the resulting maltitol hydrogenated liquid had a higher gluconic acid content and a lower maltitol content, and generated fusel alcohol other than maltitol, and the hydrogenated liquid was subjected to hydrolysis reaction of maltose by acid during the reaction to generate glucose and other substances, which further reacted with hydrogen to generate fusel alcohol other than maltitol with sorbitol as a main by-product, and the content of sorbitol was 10.2%.
Comparative example 2
Comparative example of the second method for preparing maltitol according to the invention, comprising the following steps: adding 600mL of maltose syrup into a hydrogenation kettle 1, adding 14g/L of skeleton nickel catalyst, adjusting the pH value of a reaction substrate in the hydrogenation kettle 1 to 6.0, setting the hydrogenation reaction temperature to 130 ℃, the hydrogenation reaction pressure to 9MPa, reacting for 2h, carrying out solid-liquid separation on a reaction solution in the hydrogenation kettle 1 after the hydrogenation reaction is finished, and filtering to remove the nickel catalyst to obtain a maltitol solution; wherein, 5% sodium hydroxide solution was injected into the reaction substrate at a flow rate of 3mL/min for 5min at 10min and 30min of the hydrogenation reaction, respectively. In the obtained maltitol solution, the content of gluconic acid was 1.50%, the content of maltitol was 82.5%, and the conversion of maltose was 97.5%.
In comparative example 2, the alkali injection was carried out twice in the middle stage before the hydrogenation reaction, and the alkali injection time was earlier, and a large amount of carboxylic acid by-products were again generated, which resulted in an excessively acidic environment of the reaction substrate, easily caused the isomerization reaction and the cannizzaro reaction, and affected the maltitol content in the product, wherein sorbitol was the main by-product, and the content was 8.7%.
The test data of the above examples and comparative examples are collated to give Table 1.
TABLE 1 comparative table of test data of examples 1 to 8 and comparative examples 1 to 2
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. A process for the preparation of maltitol, characterized in that it comprises the following steps:
step one, feeding: adding maltose syrup and a nickel catalyst into a hydrogenation kettle in proportion, and starting a stirring device of the hydrogenation kettle to uniformly mix reaction substrates in the hydrogenation kettle;
step two, adjusting the pH value: adjusting the initial pH value of the reaction to 5.0-6.0 by using alkali liquor with the concentration of 5%;
step three, hydrogenation: introducing hydrogen into the system obtained in the second step, controlling the temperature of the hydrogenation kettle to be 125-135 ℃ and the pressure to be 8.5-9.0 MPa, and carrying out hydrogenation reaction on a reaction substrate in the hydrogenation kettle for about 2.0-2.5 h;
step four, alkali is injected in sections: in the hydrogenation reaction process of the third step, NaOH solutions with the concentration of 5% are respectively injected into different reaction stages, and the pH value of a reaction substrate in the hydrogenation reaction is controlled to be 5.5-6.0;
step five, solid-liquid separation: after the hydrogenation reaction is finished, the reaction solution in the hydrogenation kettle is sequentially subjected to cooling, sedimentation and filtration treatment to obtain the maltitol solution.
2. The process for producing maltitol according to claim 1, wherein in the fourth step, the alkali is injected twice or three times in stages, and when the alkali is injected twice, the alkali injection time is set to 5min to 10min and 60min to 90min of the hydrogenation reaction; and when the alkali injection times are three times, the alkali injection time is arranged in the 5 th-10 th min, the 60 th-70 th min and the 75 th-90 th min of the hydrogenation reaction, wherein the alkali injection time for the second time and the alkali injection time for the third time are at least separated by more than 10 min.
3. The process for producing maltitol according to claim 1, wherein in the fourth step, the NaOH solution is stored in the lye tank in advance, the lye tank is communicated with one feed inlet of the hydrogenation reactor through a lye delivery pipe, and a flow meter for detecting the quantity of lye delivered is provided in the lye delivery pipe.
4. The process for the preparation of maltitol according to claim 1, characterized by comprising the following steps: adding 600mL of maltose syrup into a hydrogenation kettle, adding 14g/L of skeleton nickel catalyst, adjusting the pH value of a reaction substrate in the hydrogenation kettle to 5.6, setting the hydrogenation reaction temperature to 130 ℃, the hydrogenation reaction pressure to 9MPa, reacting for 2.5h, carrying out solid-liquid separation on a reaction solution in the hydrogenation kettle after the hydrogenation reaction is finished, and filtering to remove the nickel catalyst to obtain a maltitol solution; wherein, at the 10 th min and the 60 th min of the hydrogenation reaction, 5 percent sodium hydroxide solution is respectively injected into the reaction substrate at the flow rate of 3mL/min for 5 min; the pH of the reaction substrate was controlled to 5.7.
5. The process for the preparation of maltitol according to claim 1, characterized by comprising the following steps: adding 600mL of maltose syrup into a hydrogenation kettle, adding 14g/L of skeleton nickel catalyst, adjusting the pH value of a reaction substrate in the hydrogenation kettle to 5.8, setting the hydrogenation reaction temperature to 130 ℃, the hydrogenation reaction pressure to 9MPa, reacting for 2.5h, carrying out solid-liquid separation on a reaction solution in the hydrogenation kettle after the hydrogenation reaction is finished, and filtering to remove the nickel catalyst to obtain a maltitol solution; wherein, at the 10 th min and the 90 th min of the hydrogenation reaction, 5% sodium hydroxide solution is respectively injected into the reaction substrate at the flow rate of 3mL/min for 5min, and the pH value of the reaction substrate is controlled to be 5.9.
6. The process for the preparation of maltitol according to claim 1, characterized by comprising the following steps: adding 600mL of maltose syrup into a hydrogenation kettle, adding 14g/L of skeleton nickel catalyst, adjusting the pH value of a reaction substrate in the hydrogenation kettle to 5.8, setting the hydrogenation reaction temperature to 130 ℃, the hydrogenation reaction pressure to 9MPa, reacting for 2.5h, carrying out solid-liquid separation on a reaction solution in the hydrogenation kettle after the hydrogenation reaction is finished, and filtering to remove the nickel catalyst to obtain a maltitol solution; wherein, 5% sodium hydroxide solution is respectively injected into the reaction substrate for 5min at the flow rate of 3mL/min at the 10 th min, the 60 th min and the 75 th min of the hydrogenation reaction; the pH of the reaction substrate was controlled to 5.9.
7. The process for the preparation of maltitol according to claim 1, characterized by comprising the following steps: adding 600mL of maltose syrup into a hydrogenation kettle, adding 14g/L of skeleton nickel catalyst, adjusting the pH value of a reaction substrate in the hydrogenation kettle to 5.5, setting the hydrogenation reaction temperature to 130 ℃, the hydrogenation reaction pressure to 8.5MPa, reacting for 2.5h, carrying out solid-liquid separation on a reaction solution in the hydrogenation kettle after the hydrogenation reaction is finished, and filtering to remove the nickel catalyst to obtain a maltitol solution; wherein, 5% sodium hydroxide solution is respectively injected into the reaction substrate for 5min at the flow rate of 3mL/min at the 10 th min, the 60 th min and the 90 th min of the hydrogenation reaction; the pH of the reaction substrate was controlled to 5.6.
8. The process for the preparation of maltitol according to claim 1, characterized by comprising the following steps: adding 3L of maltose syrup into a hydrogenation kettle, adding 14g/L of skeleton nickel catalyst, adjusting the pH value of a reaction substrate in the hydrogenation kettle to 5.6, setting the hydrogenation reaction temperature to 130 ℃, the hydrogenation reaction pressure to 9MPa, reacting for 2h, carrying out solid-liquid separation on a reaction solution in the hydrogenation kettle after the hydrogenation reaction is finished, and filtering to remove the nickel catalyst to obtain a maltitol solution; wherein, 5% sodium hydroxide solution is respectively injected into the reaction substrate for 5min at the flow rate of 15mL/min at the 10 th min and the 90 th min of the hydrogenation reaction; the pH of the reaction substrate was controlled to 5.7.
9. The process for the preparation of maltitol according to claim 1, characterized by comprising the following steps: adding 3L of maltose syrup into a hydrogenation kettle, adding 14g/L of a skeletal nickel catalyst, adjusting the pH value of a reaction substrate in the hydrogenation kettle to 5.7, setting the hydrogenation reaction temperature to 130 ℃, the hydrogenation reaction pressure to 8.5MPa, reacting for 2 hours, carrying out solid-liquid separation on a reaction solution in the hydrogenation kettle after the hydrogenation reaction is finished, and filtering to remove the nickel catalyst to obtain a maltitol solution; wherein, 5% sodium hydroxide solution is respectively injected into the reaction solution for 5min at the flow rate of 15mL/min at the 10 th min, the 60 th min and the 90 th min of the hydrogenation reaction; the pH of the reaction substrate was controlled to 5.8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210701944.6A CN114989230A (en) | 2022-06-20 | 2022-06-20 | Method for preparing maltitol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210701944.6A CN114989230A (en) | 2022-06-20 | 2022-06-20 | Method for preparing maltitol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114989230A true CN114989230A (en) | 2022-09-02 |
Family
ID=83037099
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210701944.6A Pending CN114989230A (en) | 2022-06-20 | 2022-06-20 | Method for preparing maltitol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114989230A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB838766A (en) * | 1957-07-02 | 1960-06-22 | Udic Sa | A process for the production of polyhydric alcohol mixtures by degradative hydrogenation of sugars |
| CN105561894A (en) * | 2016-02-24 | 2016-05-11 | 浙江华康药业股份有限公司 | Self-organization flow division type control method and device for preparing sorbitol through integral reaction and separation |
| CN109336939A (en) * | 2018-12-01 | 2019-02-15 | 浙江华康药业股份有限公司 | A kind of hydrogenation process of sugar alcohol |
| CN110845303A (en) * | 2019-11-30 | 2020-02-28 | 浙江华康药业股份有限公司 | Method for improving glucose hydrogenation efficiency |
| CN113956301A (en) * | 2021-11-24 | 2022-01-21 | 浙江大学 | Multi-kettle series continuous hydrogenation method and device for sugar alcohol production |
-
2022
- 2022-06-20 CN CN202210701944.6A patent/CN114989230A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB838766A (en) * | 1957-07-02 | 1960-06-22 | Udic Sa | A process for the production of polyhydric alcohol mixtures by degradative hydrogenation of sugars |
| CN105561894A (en) * | 2016-02-24 | 2016-05-11 | 浙江华康药业股份有限公司 | Self-organization flow division type control method and device for preparing sorbitol through integral reaction and separation |
| CN109336939A (en) * | 2018-12-01 | 2019-02-15 | 浙江华康药业股份有限公司 | A kind of hydrogenation process of sugar alcohol |
| CN110845303A (en) * | 2019-11-30 | 2020-02-28 | 浙江华康药业股份有限公司 | Method for improving glucose hydrogenation efficiency |
| CN113956301A (en) * | 2021-11-24 | 2022-01-21 | 浙江大学 | Multi-kettle series continuous hydrogenation method and device for sugar alcohol production |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103508878B (en) | A kind of method of being prepared high purity ethanol acid crystal by methyl glycollate | |
| CN114315767A (en) | Preparation method and preparation device of 5-hydroxymethylfurfural | |
| CN113956301A (en) | Multi-kettle series continuous hydrogenation method and device for sugar alcohol production | |
| CN111545213A (en) | Acid-resistant alloy catalyst | |
| EP2487224B1 (en) | Process for hydrolysis and catalytic treatment of lignocellulose biomass to produce bio-gasoline | |
| CN114989230A (en) | Method for preparing maltitol | |
| CN219636905U (en) | Acid-catalyzed sodium borohydride solution hydrolysis hydrogen production device | |
| CN102070693A (en) | Method for preparing ursodesoxycholic acid by chiral catalytic hydrogenation of 7-ketodesoxycholic acid | |
| CN109704917B (en) | Process for chemically converting corncob furfural residues into bioethanol | |
| CN103012065B (en) | Method for preparing high-concentration polyhydric alcohol by circularly hydrolyzing and hydrogenating biomass | |
| CN213708188U (en) | Device for synthesizing cyclohexanol from cyclohexene | |
| CN115215752A (en) | Method and equipment for preparing dopamine substance by using papermaking black liquor | |
| CN111116407B (en) | Method for preparing DCB reducing substance by continuous catalytic hydrogenation reduction | |
| CN1911901A (en) | Production technology of formamide | |
| JP2013135615A (en) | Biomass saccharification method | |
| CN106748772A (en) | A kind of production method of methyl acetate | |
| CN216756367U (en) | 2-hydroxyl tetrahydrofuran continuous production device | |
| CN114835571B (en) | Method and system for synthesizing succinic acid by ethylene glycol dicarbonylation | |
| CN101168520A (en) | Method for producing 1,1'-phenylsulfonyl-4,4'-diallyl (2) ether | |
| CN115594565B (en) | Process for preparing 1, 3-propylene glycol by glycerol hydrogenation | |
| CN102391065A (en) | Method for producing dihydric alcohol and low molecular polyalcohol by taking corn husk as raw material | |
| CN215828659U (en) | Device for continuously hydrolyzing ethylene carbonate | |
| CN113004226B (en) | Method for continuously synthesizing epichlorohydrin based on reaction control phase transfer catalysis system | |
| CN220056681U (en) | System for isononanoic acid is prepared in isononanal oxidation | |
| CN101914004B (en) | Synthesis process of calcium formate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |