CN217774134U - System for continuously separating hydrogenated sugar liquid - Google Patents

Abstract

The utility model relates to a system for continuous separation hydrogenation sugar liquid, include the hydrogenation cauldron through the pipeline intercommunication, the catalyst recovery cauldron, first filtration system, second filtration system, the crude jar, the backwash jar, first delivery pump, second delivery pump and third delivery pump, first filtration system and second filtration system parallelly connected respectively with first delivery pump, the cauldron is retrieved to the catalyst, crude jar and backwash jar intercommunication, first delivery pump and hydrogenation cauldron intercommunication, second delivery pump one end and hydrogenation cauldron intercommunication, its other end and catalyst recovery cauldron intercommunication, backwash jar and third delivery pump intercommunication. The utility model realizes the rapid and effective separation of the catalyst in the hydrogenation liquid, and can obviously reduce the loss of the catalyst; secondly, the load of refining processes such as subsequent decolorization, ion exchange and the like can be obviously reduced; meanwhile, the system is simple, the investment is low, and the production cost can be effectively reduced.

Description

System for continuously separating hydrogenated sugar liquid

Technical Field

The utility model belongs to the technical field of the sugar alcohol preparation, in particular to system for continuously separating hydrogenated sugar liquid.

Background

At present, the production process of sugar alcohol at home and abroad comprises the steps of hydrolysis sugar preparation, catalytic hydrogenation, filtration and decolorization, ion exchange, evaporative crystallization and the like, wherein the catalytic hydrogenation is a key process. The hydrogenation process mainly adopts an intermittent kettle to carry out hydrogenation reduction on sugar liquor by utilizing a metal catalyst under high temperature and high pressure to obtain hydrogenated sugar liquor, and then the hydrogenated sugar liquor is separated to obtain a sugar alcohol crude product and a catalyst, wherein the sugar alcohol crude product is refined in the next step, the catalyst is returned to a reaction system to be recycled, and the quality of the separation effect in the process is a key factor influencing the subsequent refining of the sugar alcohol. For example, patent publication No. CN112264111A provides a system and method for recovering activity of a glucose hydrogenation catalyst, in which a primary settling tank and a secondary settling tank are used to separate the catalyst, and the process adopts a two-stage natural settling manner to treat a glucose hydrogenation solution, and has long standing time, incomplete catalyst settling and large catalyst loss. Also, for example, patent publication No. CN201296736Y provides a separation device for a sugar solution hydrogenation catalyst, which uses a combination of an electromagnet and a settling chamber to separate the catalyst, but needs to use the electromagnet, and has the problems of high cost and high energy consumption of industrial equipment of the electromagnet.

SUMMERY OF THE UTILITY MODEL

The technical problem to be solved by the utility model is to provide a system for continuously separating hydrogenated sugar solution, which realizes the rapid and effective separation of the catalyst in the hydrogenated sugar solution and can obviously reduce the loss of the catalyst; secondly, the load of refining processes such as subsequent decolorization, ion exchange and the like can be obviously reduced; meanwhile, the system is simple, the investment is low, and the production cost can be effectively reduced.

The utility model discloses a realize like this, the utility model provides a system of continuous separation hydrogenation sugar liquid, include the hydrogenation cauldron through the pipeline intercommunication, the cauldron is retrieved to the catalyst, first filtration system, the second filtration system, the crude jar, the backwash jar, first delivery pump, second delivery pump and third delivery pump, wherein, in first filtration system and second filtration system, one is in filtering operation state, another then is in standby state, the discharge gate of hydrogenation cauldron is through first delivery pump respectively with first filtration system, the lower part feed inlet intercommunication of second filtration system, first filtration system and second filtration system are used for filtering the interior hydrogenated liquid of carrying of hydrogenation cauldron respectively, first filtration system and second filtration system's bottom discharge gate communicates with the feed inlet of catalyst recovery cauldron respectively, the upper portion discharge gate of first filtration system and second filtration system communicates with the feed inlet of second crude respectively, the crude jar is arranged in keeping in the filtration cauldron rich in the sugar alcohol component's that obtains sugar alcohol crude solution through first filtration system and second filtration system's feed inlet, the lower part discharge gate of backwash jar passes through the third delivery pump respectively with the feed inlet of second filtration system, the inside wash liquor that the filtration system was carried the catalyst contained the second filtration cauldron and was linked through the backwash jar, the top of catalyst recovery cauldron.

Further, the sugar alcohol crude product solution is a solution rich in any one of xylitol, sorbitol, maltitol and mannitol.

Further, the catalyst is a nickel catalyst.

Compared with the prior art, the system for continuously separating the hydrogenated sugar liquid has the following characteristics:

1. can continuously treat hydrogenated liquid, quickly realize the separation and the recycling of the catalyst, and the content of the catalyst in the separated sugar alcohol crude product is less than or equal to 0.1g/L.

2. The loss of the catalyst is less than or equal to 0.15kg/T (based on the dry basis of the product), the loss rate of the catalyst can be reduced by 25 percent, the recovery rate of the catalyst is more than or equal to 99 percent, the load of the subsequent refining processes such as decolorization, ion exchange and the like is further reduced, the electric conductivity of the sugar alcohol hydrogenated liquid after decolorization and ion exchange is less than 15 mu s/cm, and the light transmittance of the liquid is more than 99 percent.

3. The continuous separation process can shorten the separation time to be less than 2h and improve the separation efficiency.

Drawings

FIG. 1 is a schematic diagram of the structure of a preferred embodiment of the present invention.

Detailed Description

In order to make the technical problem, technical solution and advantageous effects to be solved by the present invention more clearly understood, the following description is given in conjunction with the accompanying drawings and embodiments to illustrate the present invention in further detail. 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 present invention is shown in the system for continuously separating hydrogenated sugar solution, wherein the arrows indicate the flowing direction of the material flows (including hydrogenated liquid, crude sugar alcohol solution, backwash water, etc.) in the system. The system for continuously separating the hydrogenated sugar solution comprises a hydrogenation kettle 1, a catalyst recovery kettle 2, a first filtering system 3, a second filtering system 4, a crude product tank 5, a backwashing tank 6, a first delivery pump 7, a second delivery pump 8 and a third delivery pump 9 which are communicated through pipelines, wherein one of the first filtering system 3 and the second filtering system 4 is in a filtering working state, and the other one is in a standby state. Necessary valves are provided in the respective pipes for ensuring the direction of the system flow, and the valves are not shown in the figure only for the sake of simplicity, and do not represent that no valves are provided.

The discharge port of the hydrogenation kettle 1 is respectively communicated with the lower feed ports of the first filtering system 3 and the second filtering system 4 through a first delivery pump 7. The first filtering system 3 and the second filtering system 4 are respectively used for filtering the hydrogenated liquid conveyed from the hydrogenation kettle. The bottom discharge ports of the first filtering system 3 and the second filtering system 4 are respectively communicated with the feed inlet of the catalyst recovery kettle 2, and the upper discharge ports of the first filtering system 3 and the second filtering system 4 are respectively communicated with the feed inlet of the crude product tank 5. The crude tank 5 serves to temporarily store the sugar alcohol crude solution enriched in the sugar alcohol component obtained by filtration through the first filtration system 3 and the second filtration system 4. The crude sugar alcohol solution is used for subsequent refining.

A discharge port at the lower part of the backwashing tank 6 is respectively communicated with feed ports at the tops of the first filtering system 3 and the second filtering system 4 through a third delivery pump 9, backwashing water in the backwashing tank 6 respectively washes the catalyst intercepted by the first filtering system 3 and the second filtering system 4, and the backwashing water containing the catalyst is delivered to the catalyst recovery kettle 2 for storage. The discharge port of the catalyst recovery kettle 2 is communicated with the feed port of the hydrogenation kettle 1 through a second conveying pump 8, and the backwash liquid containing the catalyst is conveyed into the hydrogenation kettle 1 by the second conveying pump 8 to be reused.

The sugar alcohol crude product solution is a solution rich in any one of xylitol, sorbitol, maltitol and mannitol.

The catalyst is a nickel catalyst.

The working principle of the system for continuously separating hydrogenated sugar solution according to the present invention will be further described with reference to the following specific examples.

Example 1

This example illustrates a first example of a xylitol hydrogenation solution separation and refining process using the system for continuously separating a hydrogenated sugar solution according to the present invention, which includes the following steps:

and 11, adding the skeletal nickel catalyst and the xylose raw material into a hydrogenation kettle 1 according to the proportion of 12g/L, and carrying out xylose hydrogenation reaction under the conditions of reaction temperature of 120 ℃, hydrogen pressure of 8MPa and reaction time of 1.5h, wherein the content of xylitol in the generated xylitol hydrogenation liquid is 98.5%.

And step 12, conveying the hydrogenated xylitol liquid after hydrogenation to the first filtering system 3 for filtering and separating treatment through the first conveying pump 7 according to the flow rate of 18 m/h. The feeding temperature of the hydrogenation liquid is 85 ℃, the feeding pressure is 0.2MPa, the filtering area of the first filtering system 3 is 12 square meters, the number of the filter elements is 30, the precision of the filter elements is 5 mu m, and the filtering time is 1.5h. The xylitol hydrogenation liquid is separated by a first filtering system 3 to obtain a xylitol crude product solution, wherein the Ni content is 0.06g/L, the pH value is 5.8, the electric conductance is 85 mus/cm, and the light transmission of the feed liquid is 90%.

And step 13, feeding the obtained xylitol crude product solution into a decoloring kettle for decoloring to obtain a xylitol decoloring solution. The conditions of the decoloring treatment are as follows: decolorizing at 60 deg.C for 1.5h. The pH value of the decolorized solution of the xylitol is 5.9, the electric conductivity value is reduced to 56 mu s/cm, and the light transmission of the feed liquid is 95 percent. And (3) subjecting the decolorized xylitol solution to ion exchange treatment to obtain an ion exchange xylitol solution, wherein the discharge conductance of the ion exchange xylitol solution is 10 mu s/cm, and the liquid material transmittance is 99.4%.

And step 14, when the first filtering system 3 stops being used, carrying out backwashing operation on the first filtering system 3 by backwashing water in the backwashing tank 6 according to the flow rate of 2 m/h, the flushing pressure of 0.5MPa and the flushing time of 2h, and measuring the Ni content in the backwashing liquid recovered by the catalyst recovery kettle 2 to be 85.50g/L after backwashing is finished. And conveying the backwash liquid into the hydrogenation kettle 1 through a second conveying pump 8, adding 0.06g/L of fresh Ni catalyst (for xylose raw material), and carrying out a new batch of xylose hydrogenation reaction under the conditions of reaction temperature of 120 ℃, hydrogen pressure of 9MPa and reaction time of 2h to generate a new batch of xylitol hydrogenation liquid, and repeating the steps without repeated description.

Example 2

This example illustrates a second example of a process for separating and purifying a maltitol hydrogenated liquid using the system for continuously separating a hydrogenated sugar liquid according to the present invention, by taking a process for treating a maltitol hydrogenated liquid as an example, comprising the steps of:

step 21, adding the skeletal nickel catalyst and the maltose raw material into a hydrogenation kettle 1 according to the proportion of 14g/L, and carrying out maltose hydrogenation reaction under the conditions of reaction temperature of 120 ℃, hydrogen pressure of 10MPa and reaction time of 2h, wherein the content of maltitol in the generated maltitol hydrogenated liquid is 88.5%.

And 22, conveying the hydrogenated maltitol solution to the first filtering system 3 through the first conveying pump 7 at the flow rate of 20 m/h for filtering and separating the maltitol solution after hydrogenation. The feeding temperature of the hydrogenation liquid is 90 ℃, the feeding pressure is 0.3MPa, the filtering area of the first filtering system 3 is 12 square meters, the number of filter elements is 30, the precision of the filter elements is 5 mu m, and the filtering time is 2h. The maltitol hydrogenated liquid is separated by the first filtering system 3 to obtain a maltitol crude product solution, wherein the Ni content is 0.05g/L, the pH value is 5.8, the electric conductivity is 95 mus/cm, and the light transmittance of the feed liquid is 88%.

And step 23, feeding the obtained maltitol crude product solution into a decoloring kettle for decoloring to obtain a maltitol decoloring solution. The conditions of the decoloring treatment are as follows: decolorizing at 60 deg.C for 1.5h. The pH of the maltitol decoloring solution is 5.9, the electric conductivity value is reduced to 60 mu s/cm, and the light transmittance of the feed liquid is 94 percent. Subjecting the decolorized solution to ion exchange treatment to obtain maltitol ion exchange solution, discharging the maltitol ion exchange solution, wherein the conductance is 13 mus/cm, and the liquid material transmittance is 99.1%.

And 24, when the first filtering system 3 stops being used, carrying out backwashing operation on the first filtering system 3 by backwashing water in the backwashing tank 6 according to the flow rate of 2 m/h, the flushing pressure of 0.5MPa and the flushing time of 2h, and measuring the Ni content in the backwashing liquid recovered by the catalyst recovery kettle 2 to be 100.49g/L after backwashing is finished. The backwash liquid is conveyed into the hydrogenation kettle 1 through a second conveying pump 8, 0.06g/L of fresh Ni catalyst (for maltose raw material) is added, a new batch of maltitol hydrogenation reaction is carried out under the conditions of reaction temperature of 120 ℃, hydrogen pressure of 10MPa and reaction time of 2h, a new batch of xylitol hydrogenation liquid is generated, and the steps are repeated without repeated description.

The above description is only exemplary of the present invention and should not be taken as limiting the scope of the present invention, as any modifications, equivalents, improvements and the like made within the spirit and principles of the present invention are intended to be included within the scope of the present invention.

Claims (3)

1. A system for continuously separating hydrogenated sugar solution is characterized by comprising a hydrogenation kettle, a catalyst recovery kettle, a first filtering system, a second filtering system, a crude product tank, a backwashing tank, a first conveying pump, a second conveying pump and a third conveying pump which are communicated through a pipeline, wherein one of the first filtering system and the second filtering system is in a filtering working state, the other one of the first filtering system and the second filtering system is in a standby state, a discharge port of the hydrogenation kettle is respectively communicated with a lower feed port of the first filtering system and a lower feed port of the second filtering system through the first conveying pump, the first filtering system and the second filtering system are respectively used for filtering hydrogenated liquid conveyed from the hydrogenation kettle, bottom discharge ports of the first filtering system and the second filtering system are respectively communicated with a feed port of the catalyst recovery kettle, upper discharge ports of the first filtering system and the second filtering system are respectively communicated with a feed port of the crude product tank, the first filtering system and the second filtering system are used for temporarily storing sugar alcohol solution rich in sugar alcohol components obtained by filtering the crude product through the first filtering system and the second filtering system, a lower discharge port of the backwashing tank is respectively communicated with the feed port of the first filtering system and the catalyst containing the catalyst, and the backwashing liquid conveyed to the second filtering system through the feed port of the second filtering system, and the backwashing liquid, and the catalyst recovery kettle through the second conveying system, and the discharge port of the catalyst recovery kettle, and the backwashing liquid containing the catalyst recovery kettle through the second conveying system, and the catalyst recovery kettle, and the discharge port of the catalyst recovery kettle, and the backwashing liquid containing the catalyst recovery kettle.

2. The system for continuously separating a hydrogenated sugar solution according to claim 1, wherein said crude sugar alcohol solution is a solution rich in any one of xylitol, sorbitol, maltitol, and mannitol.

3. The system for continuously separating a hydrogenated sugar solution according to claim 1, wherein said catalyst is a nickel catalyst.

Images