TWI642629B - Method for treating process water - Google Patents
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- TWI642629B TWI642629B TW104126165A TW104126165A TWI642629B TW I642629 B TWI642629 B TW I642629B TW 104126165 A TW104126165 A TW 104126165A TW 104126165 A TW104126165 A TW 104126165A TW I642629 B TWI642629 B TW I642629B
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- 238000000034 method Methods 0.000 title claims abstract description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000001914 filtration Methods 0.000 claims abstract description 49
- 238000000605 extraction Methods 0.000 claims abstract description 18
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000003763 carbonization Methods 0.000 claims abstract description 11
- NOEGNKMFWQHSLB-UHFFFAOYSA-N 5-hydroxymethylfurfural Chemical compound OCC1=CC=C(C=O)O1 NOEGNKMFWQHSLB-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003864 humus Substances 0.000 claims abstract description 8
- RJGBSYZFOCAGQY-UHFFFAOYSA-N hydroxymethylfurfural Natural products COC1=CC=C(C=O)O1 RJGBSYZFOCAGQY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims description 30
- 239000012466 permeate Substances 0.000 claims description 25
- 239000012465 retentate Substances 0.000 claims description 10
- JOOXCMJARBKPKM-UHFFFAOYSA-N 4-oxopentanoic acid Chemical compound CC(=O)CCC(O)=O JOOXCMJARBKPKM-UHFFFAOYSA-N 0.000 claims description 6
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 6
- 239000008103 glucose Substances 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 6
- 229930091371 Fructose Natural products 0.000 claims description 4
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 4
- 239000005715 Fructose Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000012216 screening Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 15
- 230000002452 interceptive effect Effects 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 238000004140 cleaning Methods 0.000 abstract description 3
- OQLZINXFSUDMHM-UHFFFAOYSA-N Acetamidine Chemical compound CC(N)=N OQLZINXFSUDMHM-UHFFFAOYSA-N 0.000 abstract description 2
- 239000012620 biological material Substances 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- 238000000926 separation method Methods 0.000 description 8
- 238000005374 membrane filtration Methods 0.000 description 3
- 235000000346 sugar Nutrition 0.000 description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000000717 retained effect Effects 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 240000008892 Helianthus tuberosus Species 0.000 description 1
- 235000003230 Helianthus tuberosus Nutrition 0.000 description 1
- 239000003011 anion exchange membrane Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000011086 high cleaning Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011110 re-filtration Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/38—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with substituted hydrocarbon radicals attached to ring carbon atoms
- C07D307/40—Radicals substituted by oxygen atoms
- C07D307/46—Doubly bound oxygen atoms, or two oxygen atoms singly bound to the same carbon atom
- C07D307/48—Furfural
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2311/00—Details relating to membrane separation process operations and control
- B01D2311/26—Further operations combined with membrane separation processes
- B01D2311/263—Chemical reaction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2313/00—Details relating to membrane modules or apparatus
- B01D2313/22—Cooling or heating elements
- B01D2313/221—Heat exchangers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2315/00—Details relating to the membrane module operation
- B01D2315/16—Diafiltration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2317/00—Membrane module arrangements within a plant or an apparatus
- B01D2317/02—Elements in series
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2317/00—Membrane module arrangements within a plant or an apparatus
- B01D2317/02—Elements in series
- B01D2317/022—Reject series
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2317/00—Membrane module arrangements within a plant or an apparatus
- B01D2317/02—Elements in series
- B01D2317/025—Permeate series
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/26—Treatment of water, waste water, or sewage by extraction
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
- C02F2103/365—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds from petrochemical industry (e.g. refineries)
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- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L9/00—Treating solid fuels to improve their combustion
- C10L9/08—Treating solid fuels to improve their combustion by heat treatments, e.g. calcining
- C10L9/086—Hydrothermal carbonization
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- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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- Combustion & Propulsion (AREA)
Abstract
在對生物物料進行水熱碳化的產物範圍內，除了主產物碳，還產生平臺化學品（Plattformchemkalie）：5-羥甲基糠醛以及糠醛和乙醯丙酸。這些產物要從碳化反應的工藝用水中萃取。但此時出現了這樣的問題，即，腐殖質會沉積在萃取塔的容器壁上並且要通過大的清潔耗費才能重新清除掉。此外，低聚物還會使產物的純度明顯惡化。這個問題通過一種級聯式過濾裝置來解決，工藝用水在萃取之前通過所述級聯式過濾裝置。這裏，首先在第一過濾級中除去所述干擾物質，在第二過濾級中將剩餘的產物和離析物分離。只將產物供應給萃取塔。
Description
本發明涉及一種用於特別是在萃取/提取反應產物的預備階段處理工藝用水的方法。
在水熱碳化中，在反應容器中添加蒸汽的情況下，在約150-230°C的溫度範圍內並且在約4-28bar的高壓下使生物材料碳化。除了由此形成的生物碳，還在這個過程中出現其他產物，例如特別是化工品5-羥甲基糠醛、糠醛和乙醯丙酸。在後置的步驟中從工藝用水中提取這些化工品，為此工藝用水通過提取塔。
但除了實際期望的碳化反應，還發生多種副反應，從而除了希望的產物外還形成一系列腐殖質和低聚物。這裏低聚物是指由產物的單個單體組成的小的分支的鏈。這些鏈由於其形成過程在物理和化學特性上與產物具有很強的相似性並且在後面的處理步驟中不能或難以與產物分離。和同樣形成的腐殖質一樣，低聚物也構成提取物中的干擾物質，其中出現的腐殖質明顯更多。所出現的腐殖質既可能是溶解也可以能是不溶的，其中，不溶的部分由於冷卻期間在熱交換器中沉積會導致處理能力的下降以及出現雜質，從而有時必須中斷產品的製造過程，以便對熱交換器進行清潔。溶解的部分相反會干擾後續進行的產品隔離工藝步驟，特別是產物的萃取。所述腐殖質沉積在萃取塔的壁部和分離裝置上並且因此要求較高的清潔耗費，以便保持設備運行。
在這個背景下，本發明的目的是，保持萃取塔的清潔耗費低並同時改善產物純度，並由此提高產物品質，即提高要萃取的5-羥甲基糠醛、糠醛和乙醯丙酸的品質。
這通過根據申請專利範圍第1項的特徵所述的用於處理水熱碳化工藝的工藝用水的方法來實現，所述方法合理的實施形式可以由附屬項中得到。
為此，根據本發明，在進入萃取塔之前，引導工藝用水通過級聯式過濾裝置，所述級聯式過濾裝置具有多個過濾級。在每個過濾級中，工藝用水中單個顆粒尺寸超過相應過濾的可通過性的成分都降低。因此，這樣來選擇第一過濾級中的分離介質，使得作為滲餘物基本上截留干擾物質，即腐殖質和低聚物。在構成主流的滲透物中仍然包含產物5-羥甲基糠醛、糠醛和乙醯丙酸，以及包含離析物，例如果糖或葡萄糖。這特別是適用於液態的離析物。如果採用固態的離析物，例如菊芋或木塊，則這些離析物（Edukt）保留在反應器中。
第一過濾級的滲透物作為供應流供應給第二過濾級，在第二過濾級中，這樣選擇分離介質，使得離析物，主要是果糖和葡萄糖作為第二滲餘物被截留，而第二滲透物在一定程度上僅還包含產物5-羥甲基糠醛、糠醛和乙醯丙酸以及所有小於這些產物的物質。
通過這種處理方式，一次性同時解決的多個問題。通過第一過濾消除了腐殖質，所述腐殖質會污染萃取塔並因此導致過高的耗費。同樣在第一過濾時還消除了低聚物，所述低聚物會污染產物。在第一步驟中分離的果糖或葡萄糖可以重新供應給方法過程，就是說重新帶入反應器中，並在這裏在下一個通程（Durchgang）中改善生產率。
有利地可以通過可能的其他過濾級實現第二滲透物的進一步分離，從而後面的過濾級具有通過性略大於產物的尺寸或略小於產物的尺寸的分離介質，該過濾級實現了精確地濾出單個產物。這相應重要的是分子大小。
同樣也可以利用第二滲餘物進行處理。在上面列舉的級聯式過濾裝置中，最後的分離級有這樣的任務，即，通過導出反應用水提高產物或離析物的濃度。通過這個步驟能夠有效地執行後面的萃取。所形成的滲透物特別適於在級聯裝置內部回輸給前面的過濾級，從而不會將額外的物質，例如溶解的鹽、有機物或細菌在所述前面的過濾級帶入系統中，並由此進一步提高了純度。
作為各個過濾級中的分離介質優選設置膜片篩檢程式，特別優選採用溶液擴散膜片和/或離子選擇性膜片，如陽離子交換膜片或陰離子交換膜片，因為由此在減少生產原材料和輔助材料的同時可以改善生產率。
此外已經證明合理的是，工藝用水和/或滲透物向過濾級的輸入流保持均勻，因此確保了輸入流在一定程度上相當於排出流。
此外，由於工藝用水，如直接從水熱碳化的反應器中提取的工藝用水還包含所形成的生物碳，因而合理的是在工藝用水進入第一過濾級之前先將其供應給固-液過濾級。為此，優選執行表面過濾或深床過濾，這裏優選也執行膜過濾。
圖1示出簡單/單線的級聯式過濾裝置，在來自水熱碳化工藝的工藝用水1進入萃取塔之前，需要利用所述級聯式過濾裝置對所述工藝用水進行預處理。在該階段，工藝用水1已經通過了固-液過濾，這裏對於這種過濾並不感興趣，因此沒有示出，並且所述工藝用水在這種情況下進入第一過濾級2。所述第一過濾級是膜過濾級，其可通過性設計成：使得干擾物質3，如腐殖質或低聚物作為滲餘物被截留在第一過濾級2中，而產物7和離析物6，即5-羥甲基糠醛、糠醛和乙醯丙酸以及糖、糖衍生物以及這裏特別是葡萄糖在第一滲透物4中通過第一過濾級2。干擾物質3從第一過濾級2中導出並供應給其他應用或廢棄物清理步驟。包括離析物6和產物7的第一滲透物4此時供應給另一個過濾級5，該過濾級同樣構造成膜過濾級。但該第二過濾級的可通過性這樣選擇：使得離析物6被截留，而產物7再次可以通過第二過濾級5。在這種情況下，離析物6被截留並且例如重新回輸到水熱碳化的工藝過程中。帶有產物7的第二滲透物現在可以供應給萃取塔。
圖2示出圖1所示級聯式過濾裝置的一個備選方案，其中，第二滲餘物8以及第二滲透物9都供應給另一個過濾級11。通過重新過濾使得希望的物質這樣提高濃度，即，使得後面的工藝過程能夠更為有效地進行，因此，在產物7方面，萃取塔能夠更為有效地工作。所述另一個過濾級11的另一種滲透物10這裏還供應給前面的過濾級，即第一過濾級2和第二過濾級5，並由此帶來沖洗效應（Auswaschungseffekt），作為對通過過濾進行的分離過程的輔助。
因此，前面記載了一種用於對水熱碳化工藝的工藝用水進行處理的方法，在該方法的過程中，對在水熱碳化工藝中產生的工藝用水進行過濾，使得能建立高的產物純度並且同時使得相關設備得到低的污染程度，並且由此明顯改善所述方法的效率。
1‧‧‧工藝用水
2‧‧‧第一過濾級
3‧‧‧干擾物質
4‧‧‧第一滲透物
5‧‧‧第二過濾級
6‧‧‧離析物
7‧‧‧產物
8‧‧‧第二滲餘物
9‧‧‧第二滲透物
10‧‧‧一種滲透物
11‧‧‧另一個過濾級
圖1用示意圖示出具有兩個過濾級的簡單的級聯式過濾裝置；以及 圖2用示意圖示出具有三個過濾級的擴展的級聯式過濾裝置。
Claims (8)
- 一種用於處理水熱碳化工藝的工藝用水(1)的方法，其特徵在於，在第一過濾級(2)中利用膜片篩檢程式將工藝用水(1)分離成主要包含腐殖質和/或低聚物的第一滲餘物和主要包含產物(7)和離析物(6)的第一滲透物(4)，其中所述產物(7)是5-羥甲基糠醛和/或糠醛和/或乙醯丙酸，所述離析物(6)是果糖和/或葡萄糖，並利用膜片篩檢程式將第一滲透物(4)供應給第二過濾級(5)，在第二過濾級中將第一滲透物(4)分離成主要包含果糖和/或葡萄糖的第二滲餘物和主要包含5-羥甲基糠醛和/或糠醛和/或乙醯丙酸的第二滲透物(9)，此後利用萃取塔將第二滲透物(9)供應給使用萃取產物(7)的萃取步驟。
- 如申請專利範圍第1項所述之方法，其中，在將第二滲透物(9)供應給萃取步驟或供應給備選的其他應用之前，將第二滲透物供應給至少一個另外的過濾級(11)，在所述另外的過濾級中，第二滲透物(9)分離為包含各單個產物的另外的滲透物(10)和另外的滲餘物。
- 如申請專利範圍第2項所述之方法，其中，在至少一個另外的過濾級(11)中，使第二滲餘物(8)濃度升高。
- 如申請專利範圍第2項所述之方法，其中，最後的一個或多個過濾級(11)的滲透物(10)作為輸入流供應給前面的過濾級。
- 如申請專利範圍第1或2項所述之方法，其中，前後依次設置的各過濾級的區別在於，它們截留尺寸逐漸變小的分子。
- 如申請專利範圍第2項所述之方法，其中，工藝用水(1)和/或滲透物(4、9、10)向過濾級(2、5、11)的輸入流均勻地實現。
- 如申請專利範圍第6項所述之方法，其中，調整工藝用水(1)和/或滲透物(4、9、10)向過濾級(2、5、11)的輸入流，使得排出流量最大等於輸入流量。
- 如申請專利範圍第1或2項所述之方法，其中，在工藝用水(1)進入第一過濾級(2)之前，將工藝用水供應給固-液過濾級。
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| DK2990385T3 (en) | 2018-01-15 |
| ES2654962T3 (es) | 2018-02-15 |
| US9416030B2 (en) | 2016-08-16 |
| NO2681399T3 (zh) | 2018-04-07 |
| BR102015003825B1 (pt) | 2021-10-19 |
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| PL2990385T3 (pl) | 2018-04-30 |
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