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1. 发明申请

WO2023287396A1 IMPROVED PROCESS FOR TREATING LIGNIN 审中-公开
公开(公告)号：WO2023287396A1
公开(公告)日：2023-01-19
申请号：PCT/US2021/041350
申请日：2021-07-13
申请人： LIQUID LIGNIN COMPANY , LAKE, Michael, A. , BLACKBURN, John, C. , HAYDEN, J., George
发明人： LAKE, Michael, A. , BLACKBURN, John, C. , HAYDEN, J., George
IPC分类号： C07G1/00 , C08H8/00 , C08L97/00
摘要： This invention provides improvements to processes for making granular lignin from black liquor. One of the improvements is that the use of a pre-carbonation column reduces the CO2 flow into the sparger of a carbonation column. The pre-carbonation column is used to reduce the pH of the black liquor to about 12. Another improvement is that it has been found that coalescing droplets into a bulk liquid-lignin phase can be enhanced by placing the exit of the carbonation column at or slightly beneath carbonated black liquor/liquid-lignin interface. It has also been found that operating the carbonation settler at a low pressure and pumping the liquid- lignin from the carbonation settler to the acidification reactor operating at a higher pressure allows recycling the vent gas from the acidification reactor to the pre-carbonation column. The invention also provides for a vent gas absorber.

2. 发明申请

WO2014070861A1 PH-INDUCED FRACTIONATION PROCESSES FOR RECOVERY OF LIGNIN 审中-公开
标题翻译：用于恢复LIGNIN的PH诱导分离过程
公开(公告)号：WO2014070861A1
公开(公告)日：2014-05-08
申请号：PCT/US2013/067453
申请日：2013-10-30
申请人： THIES, Mark , VELEZ-GUILLEN, Julian , BLACKBURN, John, C. , LAKE, Michael, A.
发明人： THIES, Mark , VELEZ-GUILLEN, Julian , BLACKBURN, John, C. , LAKE, Michael, A.
IPC分类号： C08H7/00 , C07G1/00 , D21C11/00
CPC分类号： C07G1/00
摘要： There are provided processes for recovering a "heart-cut" liquid-lignin fraction from a lignin-containing stream such as a black liquor stream from a paper making process or the crude lignin stream within a non-destructive biomass conversion process by carbonating, acidifying and recovering the liquid-lignin fraction. The processes generally include reacting black liquor with a carefully selected amount of carbon dioxide (C02), to decrementally reduce the pH of the black liquor and produce fractions of a dense liquid-lignin precipitate at each pH decrement to about a pH of 8. The sequential reduction in pH is less than or equal to about 1.5 in most embodiments, less than 1.0 in other embodiments, and less than 0.50 in still other embodiments. It has been discovered that lignin recovered from the dense liquid-lignin precipitate at the different pH decrements can have different molecular weight ranges and/or structures. This process provides an improved lignin with a more narrow distribution of molecular weight, melt point, and chemical structure that is more suitable for high- value polymer applications.
摘要翻译：提供了从含有木质素的物流（例如来自造纸工艺的黑液流）或非破坏性生物质转化过程中的粗木质素物流中回收“心切”液体木质素部分的方法，其通过碳酸化，酸化并回收液态木质素馏分。该方法通常包括使黑液与仔细选择量的二氧化碳（CO 2）反应，以逐渐降低黑液的pH并在每个pH降低至约pH 8时产生致密的液体 - 木质素沉淀物的馏分。在大多数实施方案中，pH的连续降低小于或等于约1.5，在其它实施方案中小于1.0，在其它实施方案中小于0.50。已经发现，在不同pH降低下从致密液体木质素沉淀回收的木质素可以具有不同的分子量范围和/或结构。该方法提供了改进的木质素，其分子量，熔点和化学结构的分布更窄，更适用于高价值聚合物应用。

3. 发明申请

WO2014014910A1 ENERGY PELLET 审中-公开
标题翻译：能量片
公开(公告)号：WO2014014910A1
公开(公告)日：2014-01-23
申请号：PCT/US2013/050679
申请日：2013-07-16
申请人： LAKE, Michael, A.
发明人： LAKE, Michael, A.
IPC分类号： C10L5/44 , C10L5/14
CPC分类号： C10L5/24 , C10L5/143 , C10L5/16 , C10L5/363 , C10L5/442 , C10L5/447 , C10L9/083 , C10L2200/0469 , C10L2230/22 , C10L2290/06 , C10L2290/24 , Y02E50/10 , Y02E50/15 , Y02E50/30
摘要： A high-energy water-resistant pellet of at least 75% torrefied wood and the remainder a binder comprising from about 2% to about 20% by total weight of the pellet. The binder is a two-component system - a plasticizer, such as tall oil pitch, rosin, fatty acid, vegetable oils, animal oils and corn protein - preferably from 3% to about 20% of the binder, and lignin from about 80-97% of the binder. A durable, low dust white wood energy pellet is also provided using the same two-component binders.
摘要翻译：一种高能耐水丸，其具有至少75％的烘焙木材，其余的是粘合剂，其占丸剂总重量的约2％至约20％。粘合剂是双组分体系 - 增塑剂，例如妥尔油沥青，松香，脂肪酸，植物油，动物油和玉米蛋白，优选约3％至约20％的粘合剂，木质素约80- 97％的粘合剂。还使用相同的双组分粘合剂提供耐用的，低灰尘的白色木材能量颗粒。

4. 发明申请

WO2012161865A1 PROCESS FOR TREATING LIGNIN 审中-公开
标题翻译：处理LIGNIN的过程
公开(公告)号：WO2012161865A1
公开(公告)日：2012-11-29
申请号：PCT/US2012/031085
申请日：2012-03-29
申请人： LIQUID LIGNIN COMPANY, LLC , LAKE, Michael A. , BLACKBURN, John C.
发明人： LAKE, Michael A. , BLACKBURN, John C.
IPC分类号： D21C11/04 , C02F1/66 , C02F1/54
CPC分类号： C07G1/00 , C02F2103/28 , D21C11/0007 , D21C11/04
摘要： A process for recovery of lignin from black liquor that contains either soluble or dispersed lignin by generating a "liquid lignin" at high yield is disclosed. Soluble lignin at a high pH is precipitated by reducing the pH of the black liquor stream by countercurrent reaction with carbon dioxide, at elevated temperature and pressure, creating a heavy lignin-rich phase and a light lignin-depleted phase. The heavy lignin- rich phase is separated and washed countercurrently with a non-sulfur containing acid, such as acetic acid, to displace metal cations from the lignin, creating a low-salt lignin, which is then formed into a low-dust, high-bulk density lignin fuel pellet. If desired, an oxidation step may be used to eliminate odor for lignins having high value green chemistry applications.
摘要翻译：公开了通过以高产率产生“液态木质素”从黑液中回收含有可溶性或分散的木质素的木质素的方法。通过在升高的温度和压力下通过与二氧化碳的逆流反应来降低黑液流的pH而沉淀出高pH下的可溶性木质素，产生富含木质素的重质相和较轻的木质素贫化相。将沉淀的富含木质素的相分离并与不含硫的酸如乙酸逆流洗涤，以从木质素中置换金属阳离子，产生低盐木质素，然后将其形成低灰尘，高稠密木质素燃料丸。如果需要，可以使用氧化步骤来消除具有高价值绿色化学应用的木质素的气味。

5. 发明申请

WO2012161916A2 PROCESS FOR PRODUCING FURFURAL FROM BLACK LIQUOR 审中-公开
标题翻译：从黑色液体生产糠醛的方法
公开(公告)号：WO2012161916A2
公开(公告)日：2012-11-29
申请号：PCT/US2012/035159
申请日：2012-04-26
申请人： LIQUID LIGNIN COMPANY, LLC , LAKE, Michael A. , BLACKBURN, John C.
发明人： LAKE, Michael A. , BLACKBURN, John C.
IPC分类号： C07D307/50 , C07D307/48
CPC分类号： C07D307/50 , C07D307/48
摘要： A process for making furfural using papermaking black liquor from the kraft pulping process as a feed material. First, the lignin is removed from the black liquor by carbonizing the black liquor to a pH below pH 10 to insolubilize the lignin, neutralize NaOH and other inorganic components of the black liquor. The next step is to treat the carbonated black liquor that contains the hemicellulose to remove the high molecular weight components. In a preferred embodiment the treatment uses multiple sequential steps. The first step of the treatment is to use ultrafiltration, centrifugation or dissolved- air floatation to separate the high molecular weight components. The second filtration is to pass the hemicellulose containing black liquor stream through a nanofilter to remove low molecular weight components. The conversion of xylans in the hemicellulose- containing mixture to furfural is accomplished using a catalytic process. The xylans are converted to pentose sugars and then converted to furfural. The furfural is formed at a low concentration and then further concentrated.
摘要翻译：使用造纸黑液从硫酸盐制浆工艺制成糠醛作为原料的方法。首先，通过将黑液碳化成低于pH 10的pH将木质素从黑液中除去，以使木质素不溶解，中和黑液中的NaOH和其它无机成分。下一步是处理含有半纤维素的碳酸黑液以除去高分子量组分。在优选实施方案中，治疗使用多个连续步骤。处理的第一步是使用超滤，离心或溶解空气漂浮来分离高分子量组分。第二次过滤是将含有半纤维素的黑液流通过纳米过滤器以除去低分子量组分。木质纤维素混合物中的木聚糖转化为糠醛是使用催化方法完成的。将木聚糖转化为戊糖，然后转化为糠醛。糠醛以低浓度形成，然后进一步浓缩。

6. 发明申请

WO2015200456A1 PROCESS FOR LOWERING MOLECULAR WEIGHT OF LIQUID LIGNIN 审中-公开
标题翻译：降低液体分子量的方法
公开(公告)号：WO2015200456A1
公开(公告)日：2015-12-30
申请号：PCT/US2015/037375
申请日：2015-06-24
申请人： LAKE, Michael, A.
发明人： LAKE, Michael, A.
IPC分类号： D21H17/23
CPC分类号： D21C11/0057 , D21C11/0007
摘要： Processes and systems for lowering molecular weight of lignin generally includes first isolating a dense liquid lignin phase from black liquor and subjecting the dense liquid lignin phase to a temperature and pressure for a period of time to effect an average molecular weight distribution of the lignin. Solid lignin produced with the lowered molecular weight is then isolated. The systems and processes may further include an oxidation unit for oxidizing the black liquor and intermediate streams to remove or mitigate malodorous or toxic emissions.
摘要翻译：用于降低木质素分子量的方法和系统通常包括首先从黑液中分离致密的液体木质素相，并使密实的液体木质素相经历一段时间的温度和压力，以实现木质素的平均分子量分布。然后分离出分子量降低的固体木质素。该系统和方法还可以包括用于氧化黑液和中间物流以消除或减轻恶臭或有毒排放物的氧化装置。

7. 发明申请

WO2011037967A3 PROCESS FOR RECOVERING LIGNIN 审中-公开
标题翻译：回收木质素的方法
公开(公告)号：WO2011037967A3
公开(公告)日：2011-03-31
申请号：PCT/US2010/049773
申请日：2010-09-22
申请人： LAKE, Michael, A. , BLACKBURN, John, C.
发明人： LAKE, Michael, A. , BLACKBURN, John, C.
IPC分类号： C07G1/00 , D21C11/04 , C08L97/00
摘要： There is provided a process for recovery of lignin from a black liquor that contains either soluble or dispersed lignin, generating a "liquid lignin" at high yield. Soluble lignin at elevated pH is precipitated by reducing the pH of the black liquor stream by countercurrent reaction with carbon dioxide, at elevated temperature and pressure, creating two bulk fluid phases: a heavy lignin-rich phase and a light lignin- depleted phase. The heavy lignin-rich phase is separated and washed countercurrently with a strong acid to displace metal cations from the lignin, creating a low-salt lignin, which is then formed into a low-dust high-bulk-density lignin fuel pellet. If needed, especially for lignin recovered from kraft papermaking black-liquor streams, an oxidation step is included to eliminate negative odor for high-value green-chemistry applications.
摘要翻译：提供了从含有可溶性或分散木质素的黑液中回收木质素的方法，产生“液体木质素” 高收益。通过在升高的温度和压力下通过与二氧化碳逆流反应降低黑液流的pH来沉淀在升高的pH下的可溶木质素，产生两个本体流体相：富木质素富集相和轻质木质素贫化相。富含木素的重质相被分离出来，并用强酸逆流洗涤以从木质素中置换金属阳离子，产生低盐木质素，然后形成低灰尘高堆密度木质素燃料芯块。如果需要，特别是对于从牛皮纸造纸黑液流中回收的木质素，包括氧化步骤以消除高价值绿色化学应用中的负面气味。

8. 发明申请

WO2012161916A3 PROCESS FOR PRODUCING FURFURAL FROM BLACK LIQUOR 审中-公开
标题翻译：从黑色液体生产糠醛的方法
公开(公告)号：WO2012161916A3
公开(公告)日：2013-02-28
申请号：PCT/US2012035159
申请日：2012-04-26
申请人： LIQUID LIGNIN COMPANY LLC , LAKE MICHAEL A , BLACKBURN JOHN C
发明人： LAKE MICHAEL A , BLACKBURN JOHN C
IPC分类号： C07D307/50 , C07D307/48
CPC分类号： C07D307/50 , C07D307/48
摘要： A process for making furfural using papermaking black liquor from the kraft pulping process as a feed material. First, the lignin is removed from the black liquor by carbonizing the black liquor to a pH below pH 10 to insolubilize the lignin, neutralize NaOH and other inorganic components of the black liquor. The next step is to treat the carbonated black liquor that contains the hemicellulose to remove the high molecular weight components. In a preferred embodiment the treatment uses multiple sequential steps. The first step of the treatment is to use ultrafiltration, centrifugation or dissolved- air floatation to separate the high molecular weight components. The second filtration is to pass the hemicellulose containing black liquor stream through a nanofilter to remove low molecular weight components. The conversion of xylans in the hemicellulose- containing mixture to furfural is accomplished using a catalytic process. The xylans are converted to pentose sugars and then converted to furfural. The furfural is formed at a low concentration and then further concentrated.
摘要翻译：使用造纸黑液从硫酸盐制浆工艺制成糠醛作为原料的方法。首先，通过将黑液碳化成低于pH 10的pH将木质素从黑液中除去，以使木质素不溶解，中和黑液中的NaOH和其它无机成分。下一步是处理含有半纤维素的碳酸黑液以除去高分子量组分。在优选实施方案中，治疗使用多个连续步骤。处理的第一步是使用超滤，离心或溶解空气漂浮来分离高分子量组分。第二次过滤是将含有半纤维素的黑液流通过纳米过滤器以除去低分子量组分。木质纤维素混合物中的木聚糖转化为糠醛是使用催化方法完成的。将木聚糖转化为戊糖，然后转化为糠醛。糠醛以低浓度形成，然后进一步浓缩。

9. 发明申请

WO2011037967A2 PROCESS FOR RECOVERING LIGNIN 审中-公开
标题翻译：回收木质素的方法
公开(公告)号：WO2011037967A2
公开(公告)日：2011-03-31
申请号：PCT/US2010049773
申请日：2010-09-22
申请人： LAKE MICHAEL A , BLACKBURN JOHN C
发明人： LAKE MICHAEL A , BLACKBURN JOHN C
IPC分类号： C07G1/00 , C08L97/00 , D21C11/04
CPC分类号： C07G1/00 , C08H8/00 , C08L97/005 , D21C11/0007 , D21C11/0085
摘要： There is provided a process for recovery of lignin from a black liquor that contains either soluble or dispersed lignin, generating a "liquid lignin" at high yield. Soluble lignin at elevated pH is precipitated by reducing the pH of the black liquor stream by countercurrent reaction with carbon dioxide, at elevated temperature and pressure, creating two bulk fluid phases: a heavy lignin-rich phase and a light lignin- depleted phase. The heavy lignin-rich phase is separated and washed countercurrently with a strong acid to displace metal cations from the lignin, creating a low-salt lignin, which is then formed into a low-dust high-bulk-density lignin fuel pellet. If needed, especially for lignin recovered from kraft papermaking black-liquor streams, an oxidation step is included to eliminate negative odor for high-value green-chemistry applications.
摘要翻译：提供了从含有可溶性或分散性木质素的黑液中回收木质素的方法，以高产率生成“液体木质素”。通过在升高的温度和压力下通过与二氧化碳逆流反应降低黑液流的pH来沉淀在升高的pH下的可溶木质素，产生两个本体流体相：富木质素富集相和轻质木质素贫化相。富含木素的重质相被分离出来，并用强酸逆流洗涤以从木质素中置换金属阳离子，产生低盐木质素，然后形成低灰尘高堆密度木质素燃料芯块。如果需要，特别是对于从牛皮纸造纸黑液流中回收的木质素，包括氧化步骤以消除高价值绿色化学应用中的负面气味。

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