CN107892644A - A kind of method that xylitol is reclaimed from more subcrystalline Xylitol mother liquor - Google Patents

A kind of method that xylitol is reclaimed from more subcrystalline Xylitol mother liquor Download PDF

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Publication number
CN107892644A
CN107892644A CN201711294461.4A CN201711294461A CN107892644A CN 107892644 A CN107892644 A CN 107892644A CN 201711294461 A CN201711294461 A CN 201711294461A CN 107892644 A CN107892644 A CN 107892644A
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xylitol
mother liquor
ultrafiltration
quality
product
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CN201711294461.4A
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孙鲁
崔静
邱学良
曹玉华
黄伟红
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Shandong Futian Pharmaceutical Co Ltd
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Shandong Futian Pharmaceutical Co Ltd
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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
    • 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
    • C07C29/78—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a kind of method that xylitol is reclaimed from more subcrystalline Xylitol mother liquor, this method step are as follows：1）Xylitol mother liquor is diluted to the 10 20% of solution quality, ultrafiltration is carried out, obtains the Xylitol mother liquor after ultrafiltration；2）Xylitol mother liquor after ultrafiltration is concentrated into mass percent concentration 80 85%, the Xylitol mother liquor concentrated；3）The Xylitol mother liquor of described concentration is heated to 75 80 DEG C, then starts gradient cooling, 55 65 DEG C of addition crystal seeds is down to, when continuing to be cooled to 25 30 DEG C, is crystallized, centrifuged xylitol product and the first miscellaneous sugar liquid；4）Described xylitol product is recrystallized, obtains xylitol crystal and the second miscellaneous sugar liquid.Compared to the prior art the present invention, has the characteristics that reasonable in design, simple to operate, energy consumption is low, the cycle is short, can direct crystallization obtain xylitol crystal, the purity of xylitol is more than 99%, and yield is higher, about 35 40%.

Description

A kind of method that xylitol is reclaimed from more subcrystalline Xylitol mother liquor
Technical field
The present invention relates to functional sugar biological chemical field, specifically one kind is returned from more subcrystalline Xylitol mother liquor The method for receiving xylitol.
Background technology
Xylitol mother liquor is the byproduct for centrifuging to obtain after xylitol crystallizes, and main component is that xylitol accounts for 50%, is also had A kind of fusel such as arabite, dulcitol and sorbierite, total sugar concentration are 60% or so.It is miscellaneous because Xylitol mother liquor purity is low Matter is more, and main integrated application in fluid form, added value are low at present.And liquid is unfavorable for storing and transported, and limits wood The application of sugar alcohol mother liquor.
CN1162384 propositions xylitol solution contacts with the particulate xylitol being suspended in gas, and dry feedstock obtains Crystallite, and raw material is adjusted to agglomerated product.The technique needs special equipment investment larger.CN1733668A is proposed in xylose Potassium sorbate or sodium gluconate are added in alcohol mother liquor, is stirred, is stored at room temperature 3-7 days, is then filtered by vacuum and obtains xylose Alcohol, this method production cycle length, xylitol yield are low.
In a word, there is the problem of cycle is long or need specific equipment, and technique is tediously long, high energy consumption in process above.
The content of the invention
The technical assignment of the present invention is to provide a kind of method that xylitol is reclaimed from more subcrystalline Xylitol mother liquor.
The technical assignment of the present invention is realized in the following manner：
A kind of method that xylitol is reclaimed from more subcrystalline Xylitol mother liquor, this method step are as follows：
Step 1）Xylitol mother liquor is diluted to the 10-20% of solution quality, ultrafiltration is carried out, obtains the Xylitol mother liquor after ultrafiltration；
Step 2）Xylitol mother liquor after ultrafiltration is concentrated into mass percent concentration 80-85%, the xylitol concentrated is female Liquid；
Step 3）The Xylitol mother liquor of described concentration is heated to 75-80 DEG C, then starts gradient cooling, is down to 55- 65 DEG C of addition crystal seeds, when continuing to be cooled to 25-30 DEG C, are crystallized, centrifuged xylitol product and the first miscellaneous sugar liquid；
Step 4）Described xylitol product is recrystallized, obtains xylitol crystal and the second miscellaneous sugar liquid.
The milipore filter that described ultrafiltration uses is hollow-fibre membrane and/or poly (ether sulfone) film.
Described ultra-filtration conditions are：Temperature is 20-30 DEG C, pressure 0.5-1.0Mpa.
Described step 3）In when continuing to be cooled to 25-30 DEG C, crystallized, including, to the xylitol of described concentration Organic solvent is added in mother liquor.
Described organic solvent adds 0.5-10% of the quality for the Xylitol mother liquor quality of described concentration.
Described organic solvent is the methanol that mass percent concentration is 99.5% and/or mass percent concentration is 99.7% Ethanol.
Described step 3）In then start gradient cooling, including, gradient cooling speed be 0.5-1.5 DEG C/h.
Described step 3）In be down to 55-65 DEG C addition crystal seed, add crystal seed quality be described concentration xylitol The 0.1-1% of mother liquor quality.
Described centrifuged xylitol product and the first miscellaneous sugar liquid, including, centrifuged using butterfly centrifugal machine, centrifugation turns Speed is 2000-3000rpm.
Described step 4）It is middle to be recrystallized described xylitol product, including, described xylitol product is molten Yu Shui, crystallization solution is obtained, be heated to 75-80 DEG C, be cooled to 60-70 DEG C of addition crystal seed, temperature is down to 25-30 DEG C of progress Crystallization, obtains xylitol crystal and the second miscellaneous sugar liquid.
Compared to the prior art a kind of method that xylitol is reclaimed from more subcrystalline Xylitol mother liquor of the present invention, has Have the features such as reasonable in design, simple to operate, energy consumption is low, the cycle is short, can direct crystallization obtain xylitol crystal, the purity of xylitol For more than 99%, and yield is higher, about 35-40%.
Embodiment
Embodiment 1：
A kind of method that xylitol is reclaimed from more subcrystalline Xylitol mother liquor, this method step are as follows：
Step 1）Xylitol mother liquor is diluted to the 10% of solution quality, ultrafiltration is carried out using hollow-fibre membrane, ultra-filtration conditions are： Temperature is 20 DEG C, pressure 0.5Mpa, obtains the 1000g Xylitol mother liquors after ultrafiltration, the mass percent of wherein xylitol contains Amount 30%；
Step 2）Xylitol mother liquor after ultrafiltration is concentrated into mass percent concentration 80% with rotary vacuum evaporator, obtained dense The Xylitol mother liquor of contracting；
Step 3）The Xylitol mother liquor of described concentration is heated to 75 DEG C, then starts gradient cooling, gradient cooling speed Rate is 0.5 DEG C/h, is down to 55 DEG C of addition crystal seeds, and the quality for adding crystal seed is the Xylitol mother liquor quality of described concentration 0.5%；When continuing to be cooled to 30 DEG C, the methanol that mass percent concentration is 99.5% is added, adds quality as described concentration The 0.5% of Xylitol mother liquor quality, is crystallized, and is centrifuged afterwards using butterfly centrifugal machine, centrifugal rotational speed 2000rpm, is obtained wood Sugar alcohol product and the first miscellaneous sugar liquid, the xylitol purity 85% of xylitol product；
Step 4）Described xylitol product is recrystallized：Described xylitol product is dissolved in water, obtains crystallization solution, Be heated to 75 DEG C, be cooled to 60 DEG C of addition crystal seeds, temperature is down to 25 DEG C and crystallized, obtain 108 g xylitol crystals and Second miscellaneous sugar liquid, xylitol purity 99%, xylitol yield 36%.
Embodiment 2：
A kind of method that xylitol is reclaimed from more subcrystalline Xylitol mother liquor, this method step are as follows：
Step 1）Xylitol mother liquor is diluted to the 13% of solution quality, ultrafiltration is carried out using poly (ether sulfone) film, ultra-filtration conditions are：Temperature Spend for 23 DEG C, pressure 0.7Mpa, obtain the mass percentage content of 1000g Xylitol mother liquors, wherein xylitol after ultrafiltration 31%；
Step 2）Xylitol mother liquor after ultrafiltration is concentrated into mass percent concentration 83% with rotary vacuum evaporator, obtained dense The Xylitol mother liquor of contracting；
Step 3）The Xylitol mother liquor of described concentration is heated to 80 DEG C, then starts gradient cooling, gradient cooling speed Rate is 1 DEG C/h, is down to 60 DEG C of addition crystal seeds, and the quality for adding crystal seed is the Xylitol mother liquor quality of described concentration 0.8%；When continuing to be cooled to 28 DEG C, the ethanol that mass percent concentration is 99.7% is added, adds quality as described concentration The 0.8% of Xylitol mother liquor quality, is crystallized, and is centrifuged afterwards using butterfly centrifugal machine, centrifugal rotational speed 2500rpm, is obtained wood Sugar alcohol product and the first miscellaneous sugar liquid, the xylitol purity 87% of xylitol product；
Step 4）Described xylitol product is recrystallized：Described xylitol product is dissolved in water, obtains crystallization solution, Be heated to 80 DEG C, be cooled to 70 DEG C of addition crystal seeds, temperature is down to 30 DEG C and crystallized, obtain the g of xylitol crystal 119 and Second miscellaneous sugar liquid, xylitol purity 99%, xylitol yield 38%.
Embodiment 3：
A kind of method that xylitol is reclaimed from more subcrystalline Xylitol mother liquor, this method step are as follows：
Step 1）Xylitol mother liquor is diluted to the 20% of solution quality, ultrafiltration is carried out using hollow-fibre membrane and poly (ether sulfone) film, surpassed Filter condition is：Temperature is 30 DEG C, pressure 1.0Mpa, obtains the quality of 1000g Xylitol mother liquors, wherein xylitol after ultrafiltration Degree 33%；
Step 2）Xylitol mother liquor after ultrafiltration is concentrated into mass percent concentration 85% with rotary vacuum evaporator, obtained dense The Xylitol mother liquor of contracting；
Step 3）The Xylitol mother liquor of described concentration is heated to 80 DEG C, then starts gradient cooling, gradient cooling speed Rate is 1.5 DEG C/h, is down to 65 DEG C of addition crystal seeds, and the quality for adding crystal seed is the Xylitol mother liquor quality of described concentration 1%；When continuing to be cooled to 25 DEG C, methanol and mass percent concentration that addition mass percent concentration is 99.5% are 99.7% Ethanol, add quality for described concentration Xylitol mother liquor quality 10%, crystallized, afterwards using butterfly centrifugal machine from The heart, centrifugal rotational speed 3000rpm, obtain xylitol product and the first miscellaneous sugar liquid, the xylitol purity 90% of xylitol product；
Step 4）Described xylitol product is recrystallized：Described xylitol product is dissolved in water, obtains crystallization solution, Be heated to 78 DEG C, be cooled to 67 DEG C of addition crystal seeds, temperature is down to 28 DEG C and crystallized, obtain the g of xylitol crystal 132 and Second miscellaneous sugar liquid, xylitol purity 99%, xylitol yield 40%.
Embodiment 4：
A kind of method that xylitol is reclaimed from more subcrystalline Xylitol mother liquor, this method step are as follows：
Step 1）Xylitol mother liquor is diluted to the 19% of solution quality, ultrafiltration is carried out using hollow-fibre membrane, ultra-filtration conditions are： Temperature is 28 DEG C, pressure 0.8Mpa, obtains the mass percentage content of 10Kg Xylitol mother liquors, wherein xylitol after ultrafiltration 30%；
Step 2）Xylitol mother liquor after ultrafiltration is concentrated into mass percent concentration 80% with rotary vacuum evaporator, obtained dense The Xylitol mother liquor of contracting；
Step 3）The Xylitol mother liquor of described concentration is heated to 80 DEG C, then starts gradient cooling, gradient cooling speed Rate is 1 DEG C/h, is down to 60 DEG C of addition crystal seeds, and the quality for adding crystal seed is the Xylitol mother liquor quality of described concentration 0.5%；When continuing to be cooled to 28 DEG C, the ethanol that mass percent concentration is 99.7% is added, adds quality as described concentration The 0.6% of Xylitol mother liquor quality, is crystallized, and is centrifuged afterwards using butterfly centrifugal machine, centrifugal rotational speed 2800rpm, is obtained wood Sugar alcohol product and the first miscellaneous sugar liquid；
Step 4）Described xylitol product is recrystallized：Described xylitol product is dissolved in water, obtains crystallization solution, Be heated to 80 DEG C, be cooled to 60 DEG C of addition crystal seeds, temperature is down to 280 DEG C and crystallized, obtain xylitol crystal 1950g and Second miscellaneous sugar liquid, purity 99%, xylitol yield 65%.
By embodiment above, the those skilled in the art can readily realize the present invention.But should Work as understanding, the present invention is not limited to above-mentioned several embodiments.On the basis of disclosed embodiment, the technology The technical staff in field can be combined different technical characteristics, so as to realize different technical schemes.

Claims (10)

  1. A kind of 1. method that xylitol is reclaimed from more subcrystalline Xylitol mother liquor, it is characterised in that this method step is as follows：
    Step 1）Xylitol mother liquor is diluted to the 10-20% of solution quality, ultrafiltration is carried out, obtains the Xylitol mother liquor after ultrafiltration；
    Step 2）Xylitol mother liquor after ultrafiltration is concentrated into mass percent concentration 80-85%, the xylitol concentrated is female Liquid；
    Step 3）The Xylitol mother liquor of described concentration is heated to 75-80 DEG C, then starts gradient cooling, is down to 55- 65 DEG C of addition crystal seeds, when continuing to be cooled to 25-30 DEG C, are crystallized, centrifuged xylitol product and the first miscellaneous sugar liquid；
    Step 4）Described xylitol product is recrystallized, obtains xylitol crystal and the second miscellaneous sugar liquid.
  2. 2. according to the method for claim 1, it is characterised in that the milipore filter that described ultrafiltration uses is hollow-fibre membrane And/or poly (ether sulfone) film.
  3. 3. according to the method for claim 1, it is characterised in that described ultra-filtration conditions are：Temperature is 20-30 DEG C, pressure For 0.5-1.0Mpa.
  4. 4. according to the method for claim 1, it is characterised in that described step 3）In when continuing to be cooled to 25-30 DEG C, enter Row crystallization, including,
    Organic solvent is added into the Xylitol mother liquor of described concentration.
  5. 5. according to the method for claim 4, it is characterised in that described organic solvent adds quality as described concentration The 0.5-10% of Xylitol mother liquor quality.
  6. 6. the method according to claim 4 or 5, it is characterised in that described organic solvent is that mass percent concentration is 99.5% methanol and/or mass percent concentration is 99.7% ethanol.
  7. 7. according to the method for claim 1, it is characterised in that described step 3）In then start gradient cooling, including,
    Gradient cooling speed is 0.5-1.5 DEG C/h.
  8. 8. according to the method for claim 1, it is characterised in that described step 3）In be down to 55-65 DEG C addition crystal seed, add The quality for entering crystal seed is the 0.1-1% of the Xylitol mother liquor quality of described concentration.
  9. 9. according to the method for claim 1, it is characterised in that described centrifuged xylitol product and the first miscellaneous sugar Liquid, including,
    Centrifuged using butterfly centrifugal machine, centrifugal rotational speed 2000-3000rpm.
  10. 10. according to the method for claim 1, it is characterised in that described step 4）It is middle to enter described xylitol product Row recrystallization, including,
    Described xylitol product is dissolved in water, crystallization solution is obtained, is heated to 75-80 DEG C, is cooled to 60-70 DEG C of addition Crystal seed, temperature are down to 25-30 DEG C and crystallized, and obtain xylitol crystal and the second miscellaneous sugar liquid.
CN201711294461.4A 2017-12-08 2017-12-08 A kind of method that xylitol is reclaimed from more subcrystalline Xylitol mother liquor Pending CN107892644A (en)

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Cited By (4)

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CN111777493A (en) * 2020-08-29 2020-10-16 浙江华康药业股份有限公司 Xylitol mother liquor utilization system and method
CN112442556A (en) * 2020-12-07 2021-03-05 浙江华康药业股份有限公司 Method for reducing sugar in xylitol crystal
CN114149304A (en) * 2021-12-27 2022-03-08 浙江华康药业股份有限公司 Multistage xylitol mother liquor crystallization system and method thereof
CN116063158A (en) * 2022-12-17 2023-05-05 浙江华康药业股份有限公司 Induction nucleation crystallization method for improving anti-caking performance of xylitol

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111777493A (en) * 2020-08-29 2020-10-16 浙江华康药业股份有限公司 Xylitol mother liquor utilization system and method
CN111777493B (en) * 2020-08-29 2024-05-10 浙江华康药业股份有限公司 Xylitol mother liquor utilization system and method
CN112442556A (en) * 2020-12-07 2021-03-05 浙江华康药业股份有限公司 Method for reducing sugar in xylitol crystal
CN114149304A (en) * 2021-12-27 2022-03-08 浙江华康药业股份有限公司 Multistage xylitol mother liquor crystallization system and method thereof
CN114149304B (en) * 2021-12-27 2023-12-05 浙江华康药业股份有限公司 Crystallization system and method for multi-stage xylitol mother liquor
CN116063158A (en) * 2022-12-17 2023-05-05 浙江华康药业股份有限公司 Induction nucleation crystallization method for improving anti-caking performance of xylitol
CN116063158B (en) * 2022-12-17 2024-05-10 浙江华康药业股份有限公司 Induction nucleation crystallization method for improving anti-caking performance of xylitol

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